Chloroform → 1-Ethoxycarbonyl-1,1-difluoro-2-butyl methacrylate

HRID 602238ノート

反応式

HRID 602238 の反応式
[F:1][C:2]([F:12])([CH:8]([OH:11])[CH2:9][CH3:10])[C:3]([O:5][CH2:6][CH3:7])=[O:4].C(Cl)(Cl)Cl.[C:17](Cl)(=[O:21])[C:18]([CH3:20])=[CH2:19].C(N(CC)CC)C>O>[C:17]([O:11][CH:8]([CH2:9][CH3:10])[C:2]([C:3]([O:5][CH2:6][CH3:7])=[O:4])([F:12])[F:1])(=[O:21])[C:18]([CH3:20])=[CH2:19]

参加物

6

反応物 4

HCID 6212ChloroformHCID 8471TriethylamineHCID 13528Methacryloyl chlorideHCID 59863825Ethyl 2,2-difluoro-3-hydroxypentanoate

生成物 1

HCID 598638611-Ethoxycarbonyl-1,1-difluoro-2-butyl methacrylate収率 66%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
55 °C

実験手順

A 25 ml reactor was charged with 1.50 g (8.2 mmol) of ethyl 2,2-difluoro-3-hydroxypentanoate, 6.5 g of chloroform, 10 mg of an antioxidant NONFLEX MBP made by Seiko Chemical Co., Ltd., 1.03 g (9.9 mmol, 1.2 eq) of methacrylic chloride, and 1.25 g (12.4 mmol, 1.5 eq) of triethylamine, followed by stirring at 55° C. for 4 hours. Then, 10 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. After conducting filtration, chloroform was distilled off, thereby obtaining 2.06 g of the target 1-ethoxycarbonyl-1,1-difluoro-2-butyl methacrylate. Purity was 66%, and yield was 66%.

後処理

  1. extractionfollowed by extraction with chloroform one time
  2. washThe obtained organic layer was washed with diluted hydrochloric acid and water
  3. customby removing water with magnesium sulfate
  4. filtrationfiltration, chloroform
  5. distillationwas distilled off

出典と根拠

ORDレコード
ord-0171143915bf454db3abcb4f5b23d98e
出典データセット
uspto-grants-2011_03
特許番号
US07906269B2

反応ノート

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