Water → HCID 178493767、化合物

HRID 845515ノート

反応式

HRID 845515 の反応式
[SH:1][C:2]1[NH:6][C:5]2[CH:7]=[CH:8][C:9]([O:11][CH2:12][C:13]([F:16])([F:15])[F:14])=[CH:10][C:4]=2[N:3]=1.[Cl-].Cl[CH2:19][C:20]1[CH:25]=[C:24]([O:26][CH3:27])[C:23]([O:28][CH3:29])=[CH:22][NH+:21]=1.O>C(O)C.[OH-].[Na+]>[CH3:27][O:26][C:24]1[C:23]([O:28][CH3:29])=[CH:22][N:21]=[C:20]([CH2:19][S:1][C:2]2[NH:6][C:5]3[CH:7]=[CH:8][C:9]([O:11][CH2:12][C:13]([F:16])([F:14])[F:15])=[CH:10][C:4]=3[N:3]=2)[CH:25]=1

参加物

6

反応物 3

HCID 962WaterHCID 201313622-Chloromethyl-4,5-dimethoxypyridinium chlorideHCID 178506345HCID 178506345、化合物

生成物 1

HCID 178493767HCID 178493767、化合物

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 14798Sodium Hydroxide溶媒

実験手順

1.0 g of 2-mercapto-5-(2,2,2-trifluoroethoxy)-1H-benzimidazole is dissolved in 15 ml of ethanol and 8.5 ml of 1N sodium hydroxide solution, 0.90 g of 2-chloromethyl-4,5-dimethoxypyridinium chloride are added and the mixture is stirred for 20 hours. After addition of 30 ml of water, the mixture is extracted three times with 30 ml of methylene chloride each time, the methylene chloride phase is washed once with 5 ml of 0.1N sodium hydroxide solution, the combined organic phases are dried over magnesium sulfate and, after the drying agent has been filtered off, the filtrate is completely concentrated. 1.51 g (94% of theory) of the title compound are obtained as an amorphous solid residue of m.p. 55°-57° C.

後処理

  1. extractionthe mixture is extracted three times with 30 ml of methylene chloride each time
  2. washthe methylene chloride phase is washed once with 5 ml of 0.1N sodium hydroxide solution
  3. dry with materialthe combined organic phases are dried over magnesium sulfate
  4. filtrationafter the drying agent has been filtered off
  5. concentrationthe filtrate is completely concentrated

出典と根拠

ORDレコード
ord-6b38d607ed584f6d874e70a98ec97057
出典データセット
uspto-grants-1988_07
特許番号
US04758579

反応ノート

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