Sodium borohydride → 1,4-Bis(4-chloro-3-nitrophenyl)butane-1,4-diol

HRID 2364782

反応式

HRID 2364782 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=[O:23])[CH2:9][CH2:10][C:11]([C:13]2[CH:18]=[CH:17][C:16]([Cl:19])=[C:15]([N+:20]([O-:22])=[O:21])[CH:14]=2)=[O:12])=[CH:4][C:3]=1[N+:24]([O-:26])=[O:25].[BH4-].[Na+]>C(O)C>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([OH:23])[CH2:9][CH2:10][CH:11]([C:13]2[CH:18]=[CH:17][C:16]([Cl:19])=[C:15]([N+:20]([O-:22])=[O:21])[CH:14]=2)[OH:12])=[CH:4][C:3]=1[N+:24]([O-:26])=[O:25]

参加物

4

反応物 2

HCID 4311764Sodium borohydrideHCID 866490991,4-Bis(4-chloro-3-nitrophenyl)butane-1,4-dione

生成物 1

HCID 767088951,4-Bis(4-chloro-3-nitrophenyl)butane-1,4-diol収率 83%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
70 °C

実験手順

The product of Example 28A (5.75 g, 14.48 mmol) was dissolved in ethanol (150 mL) at room temperature and treated with sodium borohydride (1.21 g, 31.9 mmol) portionwise over 5 minutes. The solution was heated at 70° C. for 1 h and then cooled to room temperature, quenched with water, extracted into ethyl acetate, dried over sodium sulfate, and concentrated to dryness to give 4.81 g (83%) of an off-white solid.

後処理

  1. temperaturecooled to room temperature
  2. customquenched with water
  3. extractionextracted into ethyl acetate
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated to dryness

出典と根拠

ORDレコード
ord-fdc0165b3f1c47ed8985f062a66dbb02
出典データセット
uspto-grants-2014_04
特許番号
US08691938B2

関連ノート

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