Ethanol → HCID 178517499、化合物

HRID 1931409ノート

反応式

HRID 1931409 の反応式
Br[CH2:2][C:3]([C:5]1[CH:10]=[CH:9][C:8]([F:11])=[CH:7][CH:6]=1)=O.[S-:12][C:13]#[N:14].[Na+].C([OH:18])C>>[F:11][C:8]1[CH:9]=[CH:10][C:5]([C:3]2[N:14]=[C:13]([OH:18])[S:12][CH:2]=2)=[CH:6][CH:7]=1

参加物

4

反応物 3

HCID 702EthanolHCID 967492-Bromo-1-(4-fluorophenyl)ethan-1-oneHCID 516871Sodium thiocyanate

生成物 1

HCID 178517499HCID 178517499、化合物

反応条件

温度
100 °C

実験手順

1.085 g (5 mmol) of 2-bromo-1-(4-fluoro-phenyl)-ethanone and 405 mg (5 mmol) of sodium thiocyanate in 40 ml of ethanol were heated under reflux for 30 min. Then 20 ml of ethanol were distilled off, water was added, the precipitate was filtered off, 10 ml of acetic acid, 0.5 ml of water and 0.2 ml of concentrated sulfuric acid were added, and the mixture was stirred at 100° C. for 1 h. After dilution with water, the precipitated product was filtered off, washed with water and dried. Yield: 782 mg.

後処理

  1. temperatureunder reflux for 30 min
  2. distillationThen 20 ml of ethanol were distilled off
  3. additionwater was added
  4. filtrationthe precipitate was filtered off
  5. addition10 ml of acetic acid, 0.5 ml of water and 0.2 ml of concentrated sulfuric acid were added
  6. filtrationAfter dilution with water, the precipitated product was filtered off
  7. washwashed with water
  8. customdried

出典と根拠

ORDレコード
ord-2bbfaaeeca27455a9cbc468af86954ed
出典データセット
uspto-grants-2012_05
特許番号
US08188291B2

反応ノート

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