2-(3,5-二氯苯基)乙酸甲酯

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

实验步骤: A mixture sodium methoxide in methanol (28.46 g, 25%, 0.132 mol) and toluene (150 mL) was boiled with provision of a five plate Oldershaw column to remove the methanol/toluene azeotrope. The mixture was cooled to 60° C. and toluene (a volume equal to the total volume of the distillate) was added to the mixture. Dimethyl carbonate (35.95 g, 0.399 mol) was added to the reaction mixture. Methyl 3,5-dichlorobenzeneacetate (i.e. the product from Step A1b) (22.2 g, 0.101 mol) in toluene (17 mL) was added to the mixture over 70 min. When the addition was complete the mixture was stirred for a further 60 min at 60° C. The mixture was boiled and the dimethyl carbonate/methanol azeotrope was removed using the Oldershaw column. The mixture was cooled to 25° C. and acetic acid (9.5 g, 0.158 mol) was added dropwise. Water (100 mL) was added to the mixture and the organic phase separated and removed under reduced pressure. Crystallisation of the resulting residue from methanol (36 mL) gave the product as a white solid (23.9 g, 85%) melting at 72-73° C. to remove the methanol/toluene azeotrope toluene (a volume equal to the total volume of the distillate) was added to the mixture When the addition the dimethyl carbonate/methanol azeotrope was removed The mixture was cooled to 25° C. the organic phase separated removed under reduced pressure Crystallisation of the resulting residue from methanol (36 mL)

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

实验步骤: To methyl 3,5-dichlorobenzeneethanimidate hydrochloride (1:1) (i.e. the product from Step A1a) (50 g, 0.107 mol) was added to a mixture of toluene (167 mL) and water (167 mL). After 60 min the organic phase was removed, dried (MgSO4), and evaporated to give the title compound as an oil (39 g, 91%). After 60 min the organic phase was removed dried (MgSO4) evaporated

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

实验步骤: To methyl 3,5-dichlorobenzeneethanimidate hydrochloride (1:1) (i.e. the product from Step A1a) (50 g, 0.107 mol) was added to a mixture of toluene (167 mL) and water (167 mL). After 60 min the organic phase was removed, dried (MgSO4), and evaporated to give the title compound as an oil (39 g, 91%). After 60 min the organic phase was removed dried (MgSO4) evaporated

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

实验步骤: A mixture sodium methoxide in methanol (28.46 g, 25%, 0.132 mol) and toluene (150 mL) was boiled with provision of a five plate Oldershaw column to remove the methanol/toluene azeotrope. The mixture was cooled to 60° C. and toluene (a volume equal to the total volume of the distillate) was added to the mixture. Dimethyl carbonate (35.95 g, 0.399 mol) was added to the reaction mixture. Methyl 3,5-dichlorobenzeneacetate (i.e. the product from Step A1b) (22.2 g, 0.101 mol) in toluene (17 mL) was added to the mixture over 70 min. When the addition was complete the mixture was stirred for a further 60 min at 60° C. The mixture was boiled and the dimethyl carbonate/methanol azeotrope was removed using the Oldershaw column. The mixture was cooled to 25° C. and acetic acid (9.5 g, 0.158 mol) was added dropwise. Water (100 mL) was added to the mixture and the organic phase separated and removed under reduced pressure. Crystallisation of the resulting residue from methanol (36 mL) gave the product as a white solid (23.9 g, 85%) melting at 72-73° C. to remove the methanol/toluene azeotrope toluene (a volume equal to the total volume of the distillate) was added to the mixture When the addition the dimethyl carbonate/methanol azeotrope was removed The mixture was cooled to 25° C. the organic phase separated removed under reduced pressure Crystallisation of the resulting residue from methanol (36 mL)

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

实验步骤: To methyl 3,5-dichlorobenzeneethanimidate hydrochloride (1:1) (i.e. the product from Step A1a) (50 g, 0.107 mol) was added to a mixture of toluene (167 mL) and water (167 mL). After 60 min the organic phase was removed, dried (MgSO4), and evaporated to give the title compound as an oil (39 g, 91%). After 60 min the organic phase was removed dried (MgSO4) evaporated