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

HRID 1449853ノート

反応式

HRID 1449853 の反応式
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

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

反応条件

温度
-5 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-32f4c8cbd9754f00bae4701a485ca6f1
出典データセット
uspto-grants-1997_02
特許番号
US05599986

反応ノート

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