Water → 1,2-Bis(p-chlorophenyl) ethanol

HRID 902105

反応式

HRID 902105 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=[O:17])[CH2:9][C:10]2[CH:15]=[CH:14][C:13]([Cl:16])=[CH:12][CH:11]=2)=[CH:4][CH:3]=1.[BH4-].[Na+].O>CO>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([OH:17])[CH2:9][C:10]2[CH:15]=[CH:14][C:13]([Cl:16])=[CH:12][CH:11]=2)=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 962WaterHCID 5873181,2-Bis(4-chlorophenyl)ethanoneHCID 4311764Sodium borohydride

生成物 1

HCID 420561,2-Bis(p-chlorophenyl) ethanol

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
0 °C

実験手順

A solution of 1,2-di(4-chlorophenyl)ethan-1-one (known compound) and sodium borohydride in methanol is stirred at ambient temperature for about three hours. After this time, the reaction mixture is cooled, and water is carefully added to destroy excess sodium borohydride. The mixture is cooled to 0° C. and neutralized with concentrated hydrochloric acid. The mixture is concentrated under reduced pressure to remove some of the methanol. The concentrate is taken up in ethyl acetate and washed with an aqueous solution saturated with sodium chloride. The organic layer is dried with sodium sulfate, filtered, and concentrated under reduced pressure, yielding the subject compound.

後処理

  1. temperatureAfter this time, the reaction mixture is cooled
  2. customto destroy excess sodium borohydride
  3. concentrationThe mixture is concentrated under reduced pressure
  4. customto remove some of the methanol
  5. washwashed with an aqueous solution saturated with sodium chloride
  6. dry with materialThe organic layer is dried with sodium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure
  9. customyielding the subject compound

出典と根拠

ORDレコード
ord-896f01023e9145459af97ff114d04b33
出典データセット
uspto-grants-2008_04
特許番号
US07365082B2

関連ノート

読み込み中…