反応 #1269825

反応方程式

triethylamine

2,2-difluoro-3-hydroxypentanoic acid ethyl ester

chloroform

methacrylic acid chloride

→

methacrylic acid 1-ethoxycarbonyl-1,1-difluoro-2-butyl ester

収率 66.0%

溶媒

water

反応条件

後処理

1. 1
   抽出followed by extraction with chloroform one time
2. 2
   洗浄The obtained organic layer was washed with diluted hydrochloric acid and water
3. 3
   その他by removing water with magnesium sulfate
4. 4
   ろ過a filtration
5. 5
   workup.DISTILLATIONdistilling chloroform out

実験手順

A 300 mL reactor was charged with 18.0 g (98.4 mmol) of 2,2-difluoro-3-hydroxypentanoic acid ethyl ester, 78 g of chloroform, 120 mg of an antioxidant NONFLEX MBP (a product of Seiko Chemical Co., Ltd.), 12.4 g (118.8 mmol/1.2 equivalents) of methacrylic acid chloride, and 15.0 g (148.8 mmol/1.5 equivalents) of triethylamine, followed by stirring at 55° C. for 4 hours. Then, 120 g of water was added, followed by extraction with chloroform one time. The obtained organic layer was washed with diluted hydrochloric acid and water, followed by removing water with magnesium sulfate, conducting a filtration, and distilling chloroform out, thereby obtaining 24.7 g of the target methacrylic acid 1-ethoxycarbonyl-1,1-difluoro-2-butyl ester. Upon this, purity was 66%, and yield was 66%.

出典