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Sodium Hydroxide → alpha-(2,6-Dimethyl-4-carboxyphenyl)-2-chloro-5-(1-imidazolyl)benzenemethanol

HRID 543333
ノート
印刷プレビュー

反応式

HRID 543333 の反応式
[Cl:1][C:2]1[CH:20]=[CH:19][C:18]([N:21]2[CH:25]=[CH:24][N:23]=[CH:22]2)=[CH:17][C:3]=1[C:4]([C:6]1[C:11]([CH3:12])=[CH:10][C:9]([C:13]([OH:15])=[O:14])=[CH:8][C:7]=1[CH3:16])=[O:5].[OH-].[Na+].[BH4-].[Na+]>O>[CH3:16][C:7]1[CH:8]=[C:9]([C:13]([OH:15])=[O:14])[CH:10]=[C:11]([CH3:12])[C:6]=1[CH:4]([C:3]1[CH:17]=[C:18]([N:21]2[CH:25]=[CH:24][N:23]=[CH:22]2)[CH:19]=[CH:20][C:2]=1[Cl:1])[OH:5]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 4311764Sodium borohydrideHCID 202062352-Chloro-5-(1-imidazolyl)-2',6'-dimethyl-4'-carboxybenzophenone

生成物 1

HCID 13851129alpha-(2,6-Dimethyl-4-carboxyphenyl)-2-chloro-5-(1-imidazolyl)benzenemethanol収率 94.8%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a solution of 6.4 g of 2-chloro-5-(1-imidazolyl)- 2',6'-dimethyl-4'-carboxybenzophenone and 0.8 g of sodium hydroxide in 35 ml of water is added 1.4 g of sodium borohydride, and the mixture is stirred at 70°-75° C. for 3 hours. After completion of the reaction, a small amount of an insoluble substance is filtered off from the warm mixture and the filtrate is adjusted to pH 4 with concentrated hydrochloric acid under stirring at 80°-90° C. The precipitated crystals are collected by filtration under reduced pressure, washed with water and acetone and dried to give 6.1 g of α-(2,6-dimethyl-4-carboxyphenyl)-2-chloro-5-(1-imidazolyl)benzenemethanol, melting at 317°-320° C. with decomposition as white crystals.

後処理

  1. customAfter completion of the reaction
  2. filtrationa small amount of an insoluble substance is filtered off from the warm mixture
  3. stirringunder stirring at 80°-90° C
  4. filtrationThe precipitated crystals are collected by filtration under reduced pressure
  5. washwashed with water and acetone
  6. customdried

出典と根拠

ORDレコード
ord-e5dd576a9d034743b80497a2979a9425
出典データセット
uspto-grants-1987_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04661603

反応ノート

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