乙酸正丙酯

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: In a 500-ml flask, place 39.3 g (0.25 m) of 4-fluoro-2-nitrophenol (2a) and 120 ml of isopropyl alcohol and warm to 40° C. Add 1.5 g of 5% Pd/C wet with 1.5 ml of water and stir the mixture vigorously. Add a solution of 84.1 g (1.0 m) of potassium formate in 85 ml of water in drop wise over an hour keeping the temperature at 45°-53° C. Stir the mixture at 50° C. for 2.5 hrs. Add 150 ml of propyl acetate and 100 ml of water and stir for a few min. Filter off catalyst and wash with 100 ml of propyl acetate and 100 ml of water. Separate propyl acetate solution, and wash with 150 ml water and 150 ml of brine containing 1-2 g sodium hydrosulfite. Dry propyl acetate solution over magnesium sulfate and concentrate to approximately 75 ml. Add 300 ml of heptane slowly with gentle stirring. Concentrate under a reduced pressure till most of propyl acetate evaporated. Add 150 ml of heptane to resulting mush and cool in an ice bath for about an hour. Collect solid, wash with heptane, and dry in a vacuum oven to give 29.0 g (91%) of 2-amino-4-fluorophenol (3a; X=F) as gray solids. at 45°-53° C Stir the mixture at 50° C. for 2.5 hrs stir for a few min Filter off catalyst wash with 100 ml of propyl acetate and 100 ml of water Separate propyl acetate solution, and wash with 150 ml water and 150 ml of brine containing 1-2 g sodium hydrosulfite Dry propyl acetate solution over magnesium sulfate and concentrate to approximately 75 ml Add 300 ml of heptane slowly with gentle stirring Concentrate under a reduced pressure till most of propyl acetate evaporated Add 150 ml of heptane to resulting mush cool in an ice bath for about an hour Collect solid wash with heptane dry in a vacuum oven

反应条件: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: The dried high DS starch hexanoate described above (Ex. 12, 71.3 g), ethanol (65.2 g), and n-propyl acetate (65.2 g) were charged to a 500 mL round bottom flask, equipped with condenser, overhead stirrer, nitrogen blanket, thermocouple and heating mantle. The mixture was heated to 60° C. for about 1 hr. to form a transparent, low viscosity solution at 30 wt % solids in 50/50 ethanol/n-propyl acetate. were charged to a 500 mL round bottom flask equipped with condenser overhead stirrer, nitrogen blanket, thermocouple and heating mantle

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:90.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: N,N-Dimethylformamide dimethylacetal (3.6 ml) was added to a solution of ethyl 4-(4-fluorophenyl)-3-oxobutanoate (1200 mg) in n-propyl acetate (13 ml) at room temperature, and the mixture was stirred at 90° C. for four hours. The solvent was distilled off under reduced pressure, and ethanol (18 ml) was added, followed by addition of 2-propylamine (688 μl). After stirring at 60° C. for one hour, 2-propylamine (459 μl) was added and the mixture was further stirred at 60° C. for one hour. The solvent was distilled off under reduced pressure, and the residue was purified by silica gel column chromatography [chloroform:methanol=300:1->80:1 (v/v)] to give 620 mg of the title compound as an oily substance. The solvent was distilled off under reduced pressure, and ethanol (18 ml) was added followed by addition of 2-propylamine (688 μl) After stirring at 60° C. for one hour 2-propylamine (459 μl) was added the mixture was further stirred at 60° C. for one hour The solvent was distilled off under reduced pressure the residue was purified by silica gel column chromatography [chloroform:methanol=300:1->80:1 (v/v)]

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Compounds of formula I in free form and in single stereoisomeric form thus obtained may be converted into a salt by addition of an acid to the free base of a compound of formula I. E.g. a compound of formula I may be dissolved or suspended, or is obtained in dissolved or suspended form, in organic solvent, preferably a solvent or solvent mixture, such as an alcohol, e.g. methanol, ethanol; a halogenated hydrocarbon, e.g. dichloromethane; an ether, e.g. tetrahydrofuran, an acetate, such as methyl acetate, ethyl acetate, propyl acetate, isopropyl acetate; a solvent mixture of alcohol with acetate, such as methanol/isopropyl acetate, a solvent mixture of halogenated hydrocarbon with acetate, such as dichloromethane/isopropylacetate, a solvent mixture of ether with acetate, such as tetrahydrofuran/isopropyl acetate, and to the mixture obtained an acid, e.g. an organic acid or an inorganic (mineral) acid, e.g. acetic acid, lactic acid, e.g. L-lactic acid, maleic acid, is added. A compound of formula I, in the form of a salt, e.g. crystalline salt, may be obtained and may be isolated. Compounds of formula I in free form and in single stereoisomeric form thus obtained may be converted into a salt by addition of an acid to the free base of a compound of formula I E.g. a compound of formula I may be dissolved is obtained in dissolved

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Compounds of formula I in free form and in single stereoisomeric form thus obtained may be converted into a salt by addition of an acid to the free base of a compound of formula I. E.g. a compound of formula I may be dissolved or suspended, or is obtained in dissolved or suspended form, in organic solvent, preferably a solvent or solvent mixture, such as an alcohol, e.g. methanol, ethanol; a halogenated hydrocarbon, e.g. dichloromethane; an ether, e.g. tetrahydrofuran, an acetate, such as methyl acetate, ethyl acetate, propyl acetate, isopropyl acetate; a solvent mixture of alcohol with acetate, such as methanol/isopropyl acetate, a solvent mixture of halogenated hydrocarbon with acetate, such as dichloromethane/isopropylacetate, a solvent mixture of ether with acetate, such as tetrahydrofuran/isopropyl acetate, and to the mixture obtained an acid, e.g. an organic acid or an inorganic (mineral) acid, e.g. acetic acid, lactic acid, e.g. L-lactic acid, maleic acid, is added. A compound of formula I, in the form of a salt, e.g. crystalline salt, may be obtained and may be isolated. Compounds of formula I in free form and in single stereoisomeric form thus obtained may be converted into a salt by addition of an acid to the free base of a compound of formula I E.g. a compound of formula I may be dissolved is obtained in dissolved

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Compounds of formula I in free form and in single stereoisomeric form thus obtained may be converted into a salt by addition of an acid to the free base of a compound of formula I. E.g. a compound of formula I may be dissolved or suspended, or is obtained in dissolved or suspended form, in organic solvent, preferably a solvent or solvent mixture, such as an alcohol, e.g. methanol, ethanol; a halogenated hydrocarbon, e.g. dichloromethane; an ether, e.g. tetrahydrofuran, an acetate, such as methyl acetate, ethyl acetate, propyl acetate, isopropyl acetate; a solvent mixture of alcohol with acetate, such as methanol/isopropyl acetate, a solvent mixture of halogenated hydrocarbon with acetate, such as dichloromethane/isopropylacetate, a solvent mixture of ether with acetate, such as tetrahydrofuran/isopropyl acetate, and to the mixture obtained an acid, e.g. an organic acid or an inorganic (mineral) acid, e.g. acetic acid, lactic acid, e.g. L-lactic acid, maleic acid, is added. A compound of formula I, in the form of a salt, e.g. crystalline salt, may be obtained and may be isolated. Compounds of formula I in free form and in single stereoisomeric form thus obtained may be converted into a salt by addition of an acid to the free base of a compound of formula I E.g. a compound of formula I may be dissolved is obtained in dissolved

反应条件: temp:80.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Next, 5 g of the obtained polyolefin copolymer and 750 mL of dried toluene were charged into a 2000-mL SUS autoclave thoroughly purged with a nitrogen gas, and then, after the inner temperature of the autoclave was raised to 80° C., the mixture was agitated for 2 hours to dissolve the polyolefin copolymer. Thereafter, the inside of the polymerization vessel was pressurized to 0.8 MPa with ethylene. Then, a toluene solution containing 0.75 mmol of tungsten hexachloride, 7.5 mmol of propyl acetate, and 1.5 mmol of tetramethyl tin was charged into the autoclave, and the reaction was carried out for 60 minutes while maintaining the ethylene pressure at 0.8 MPa and the inner temperature at 80° C. Thereafter, 20 mL of methanol was added to terminate the reaction. After depressurized, the obtained reaction solution was passed through a column packed with 100 g of silica gel, and then the polymer was recovered from the reaction solution by precipitation in 4 L of methanol, and dried at 130° C. for 12 hours under vacuum. The yield of the obtained polyolefin polymer containing vinyl groups at both ends thereof was 3.9 g. In the composition of the polymer, the content of ethylene was 79.8% by mole, the content of propylene was 16.6% by mole, and the content of 1,3-butadiene was 3.6% by mole. The content of 1,3-butadiene contained 0.6% by mole of 1,4-addition structure, 0.5% by mole of 1,2-addition structure, 2.3% by mole of 5-membered ring structure, and 0.2% by mole of 3-membered ring structure. The terminal vinylation ratio of the polymer was 77%, and the intrinsic viscosity [η] was 0.12 dL/g. thoroughly purged with a nitrogen gas to dissolve the polyolefin copolymer was charged into the autoclave the reaction was carried out for 60 minutes at 80° C to terminate the reaction the obtained reaction solution the polymer was recovered from the reaction solution by precipitation in 4 L of methanol dried at 130° C. for 12 hours under vacuum The yield of the obtained polyolefin polymer containing vinyl groups at both ends

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Thus in a paper published in Science 113, 206 (1951) Wender, Friedel and Orchin reported that methanol was reacted with synthesis gas (1H2 :1CO) in the presence of dicobalt octacarbonyl as catalyst to produce methyl formate (2%), methyl acetate (9.0%), ethyl alcohol (38.8%), ethyl acetate (6.3%), propyl alcohol (4.7%), butyl alcohol (0.9%), methane (8.5%), propyl acetate (0.1%) and a small amount of unidentified product, the total conversion of methanol being 76.4%.