Water → (E)-1-chloro-2-(fluoromethylene)-4-(p-fluorophenyl)butane

HRID 1449853노트

반응식

HRID 1449853 반응식
C(Cl)(=O)C([Cl:4])=O.CN(C)C=O.[F:12]/[CH:13]=[C:14](\[CH2:17][CH2:18][C:19]1[CH:24]=[CH:23][C:22]([F:25])=[CH:21][CH:20]=1)/[CH2:15]O.O>C1(C)C=CC=CC=1>[Cl:4][CH2:15]/[C:14](=[CH:13]/[F:12])/[CH2:17][CH2:18][C:19]1[CH:24]=[CH:23][C:22]([F:25])=[CH:21][CH:20]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 6228DimethylformamideHCID 65578Oxalyl chlorideHCID 10943450(E)-2-(fluoromethylene)-4-(p-fluorophenyl)butan-1-ol

생성물 1

HCID 9815806(E)-1-chloro-2-(fluoromethylene)-4-(p-fluorophenyl)butane

시약·촉매·용매 1

HCID 1140Toluene용매2회

반응 조건

온도
-5 °C

실험 절차

Combine oxalyl chloride (25.2 g, 0.198 mol) and toluene (200 mL). Cool to -5° C. Add N,N-dimethylformamide (15.0 g, 0.21 mol) as a solution in toluene (20 mL). Warm to 25° C. After 30 minutes, add a solution of (E)-2-(fluoromethylene)-4-(p-fluorophenyl)butan-l-ol (24.7 g, 30% by weight in toluene, 0.124 mol). After 18 hours, add water (500 mL) and stir for 30 minutes. Separate the organic layer, dry over Na2SO4, filter, and evaporate in vacuo to give the title compound.

후처리

  1. temperatureWarm to 25° C
  2. waitAfter 18 hours
  3. customSeparate the organic layer
  4. dry with materialdry over Na2SO4
  5. filtrationfilter
  6. customevaporate in vacuo

출처 및 근거

ORD 기록
ord-32f4c8cbd9754f00bae4701a485ca6f1
출처 데이터셋
uspto-grants-1997_02
특허 번호
US05599986

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