Sodium borohydride → (1-benzyl-4-chloro-2-(4-nitrophenyl)-1H-imidazol-5-yl)methanol

HRID 1060508ノート

反応式

HRID 1060508 の反応式
[BH4-].[Na+].[CH2:3]([N:10]1[C:14]([CH:15]=[O:16])=[C:13]([Cl:17])[N:12]=[C:11]1[C:18]1[CH:23]=[CH:22][C:21]([N+:24]([O-:26])=[O:25])=[CH:20][CH:19]=1)[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1>CO>[CH2:3]([N:10]1[C:14]([CH2:15][OH:16])=[C:13]([Cl:17])[N:12]=[C:11]1[C:18]1[CH:19]=[CH:20][C:21]([N+:24]([O-:26])=[O:25])=[CH:22][CH:23]=1)[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1

参加物

4

反応物 2

HCID 4311764Sodium borohydride2 回HCID 150885051-benzyl-4-chloro-2-(4-nitrophenyl)-1H-imidazole-5-carbaldehyde

生成物 1

HCID 15088539(1-benzyl-4-chloro-2-(4-nitrophenyl)-1H-imidazol-5-yl)methanol

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Sodium borohydride (1.1 g, 29 mmole) was added in three portions to a stirred mixture of crude 1-benzyl-4-chloro-5-formyl-2-(4-nitrophenyl)imidazole (54.2 g, 88 mmole) in methanol (250 ml) at room temperature. After two hours, more sodium borohydride (0.51 g, 15 mmol) was added, the mixture was stirred for 30 minutes and the methanol was evaporated. The residue was mixed with water (250 ml) and extracted with methylene chloride (200 ml, 3×50 ml). The combined organic solutions were washed with water (2×50 ml) and dried (NaSO4) overnight.

後処理

  1. customthe methanol was evaporated
  2. additionThe residue was mixed with water (250 ml)
  3. extractionextracted with methylene chloride (200 ml, 3×50 ml)
  4. washThe combined organic solutions were washed with water (2×50 ml)
  5. dry with materialdried (NaSO4) overnight

出典と根拠

ORDレコード
ord-a8a3c381a53a47d5a21ebe2828a2b33b
出典データセット
uspto-grants-2003_02
特許番号
US06524552B2

反応ノート

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