Dimethylformamide → HCID 53396122, 화합물

HRID 552266

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HRID 552266 반응식
CN([CH:4]=[O:5])C.O=P(Cl)(Cl)[Cl:8].[F:11][C:12]([F:23])([F:22])[C:13](=O)[CH2:14][C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1>O>[Cl:8][C:13]([C:12]([F:23])([F:22])[F:11])=[C:14]([C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)[CH:4]=[O:5]

참가 물질

5

반응물 3

HCID 6228DimethylformamideHCID 24813Phosphorus oxychlorideHCID 2229581,1,1-Trifluoro-3-phenyl-2-propanone

생성물 1

HCID 53396122HCID 53396122, 화합물

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
45 °C

실험 절차

At 0° C., DMF (4.3 mL) is carefully treated with phosphoroxychloride (2.8 mL) and the mixture is stirred at rt for 20 min before 1,1,1-trifluoro-3-phenyl-propan-2-one (1.55 mL, 10 mmol) is slowly added. The reaction mixture is stirred for 2 h at 45° C. and 18 h at rt, diluted with sat. aq. Na-acetate solution (20 mL) and water (40 mL) and extracted with diethyl ether. The organic phase is separated, washed with sat. aq. NaHCO3-solution, dried over Na2SO4 and evaporated to give 3-chloro-4,4,4-trifluoro-2-phenyl-but-2-enal (2.20 g) as a pale yellow oil.

후처리

  1. additionis slowly added
  2. extractionextracted with diethyl ether
  3. customThe organic phase is separated
  4. washwashed with sat. aq. NaHCO3-solution
  5. dry with materialdried over Na2SO4
  6. customevaporated

출처 및 근거

ORD 기록
ord-d4493b7e88f2447ab65b7d7c1a38a2a3
출처 데이터셋
uspto-grants-2011_05
특허 번호
US07951794B2

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