2,2,2-Trifluoroacetaldehyde hydrate → 4,4,4-Trifluoro-2-(2,2,2-trifluoroethyl)but-2-enoic acid ethyl ester

HRID 1987563

반응식

HRID 1987563 반응식
[CH2:1]([O:3][C:4](=[O:30])[C:5](=P(C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[CH2:6][C:7]([F:10])([F:9])[F:8])[CH3:2].O.[F:32][C:33]([F:37])([F:36])[CH:34]=O>C1COCC1>[CH2:1]([O:3][C:4](=[O:30])[C:5]([CH2:6][C:7]([F:8])([F:9])[F:10])=[CH:34][C:33]([F:37])([F:36])[F:32])[CH3:2]

참가 물질

4

반응물 2

HCID 27813662,2,2-Trifluoroacetaldehyde hydrateHCID 445414244,4,4-Trifluoro-2-(triphenyl-lambda5-phosphanylidene)-butyric acid ethyl ester

생성물 1

HCID 744100564,4,4-Trifluoro-2-(2,2,2-trifluoroethyl)but-2-enoic acid ethyl ester수율 86%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
100 °C

실험 절차

To a solution of 4,4,4-trifluoro-2-(triphenyl-λ5-phosphanylidene)-butyric acid ethyl ester (2.0 g, 4.65 mmol) in THF (5 mL) was added 1 mL of trifluoroacetaldehyde hydrate (tech.). The mixture was sealed in a pressure tube and heated at 100° C. for 3.5 h. After cooling to 23° C., the reaction mixture was eluted through a pad of silica gel (100 g) and Na2SO4 with Et2O (100 mL) to remove the by-products triphenylphosphine oxide and water. The eluent was distilled to remove Et2O and to afford the product as a colorless liquid (1.0 g, 86%).

후처리

  1. customThe mixture was sealed in a pressure tube
  2. temperatureAfter cooling to 23° C.
  3. washthe reaction mixture was eluted through a pad of silica gel (100 g) and Na2SO4 with Et2O (100 mL)
  4. customto remove the by-products triphenylphosphine oxide and water
  5. distillationThe eluent was distilled
  6. customto remove Et2O

출처 및 근거

ORD 기록
ord-a92fb0d369214c15940f164f3dfbaf1c
출처 데이터셋
uspto-grants-2009_06
특허 번호
US07550629B2

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