(E)-1-乙氧基丙酸-1-烯

反应条件: temp:50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of (E)-1-ethoxyprop-1-ene (6.41 mL, 57.9 mmol) and pyridine (4.68 mL, 57.9 mmol) was added to a soln. of 2,2,2-trichloroacetyl chloride (10.53 g, 57.9 mmol) in DCM (15 mL) at −10° C. at a rate of 6-10 drops/min. After the addition was completed, the mixture was stirred at r.t for 24 hrs. Filtered, and the filtrate was concentrated in reduced pressure (at first the temperature of the water bath was r.t, after most DCM was evaporated off, water bath was warmed to 50° C. to afford (E)-1,1,1-trichloro-4-ethoxy-3-methylbut-3-en-2-one (2.55 g, 10.79 mmol, 18.64% yield). 1H-NMR (500 MHz, CDCl3): δ: 7.96 (s, 1H), 4.21 (q, J=7.1 Hz, 2H), 1.94 (s, 3H), 1.41 (t, J=7.2 Hz, 3H). This material was taken into Step G2 without further purification. was added to a soln at −10° C. After the addition Filtered the filtrate was concentrated in reduced pressure (at first the temperature of the water bath after most DCM was evaporated off

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

实验步骤: To a solution of 2,2,2-trichloroacetyl chloride (10.6 g, 6.52 mL, 58.1 mmol) in dichloromethane (15 mL) cooled to −10° C. was added a mixture of (E)-1-ethoxyprop-1-ene (5 g, 6.43 mL, 58.1 mmol) and pyridine (4.59 g, 4.7 mL, 58.1 mmol) over a period of 15 min. After the addition was complete, the mixture was stirred at RT for 16 h. The resulting precipitate was filtered and washed with dichloromethane. The filtrate was concentrated in vacuo and dried at 40° C. in high vacuum to give the product as brown semisolid (16.1 g with 80% purity, 95.8%). The crude material was used directly in the next step without any further purification. was added After the addition The resulting precipitate was filtered washed with dichloromethane The filtrate was concentrated in vacuo dried at 40° C. in high vacuum