Water → 2-((5,6-Dimethyl-1-(phenylcarbonyl)benzimidazole-2-ylthio)methyl)benzoic acid t-butyl ester

HRID 916080ノート

反応式

HRID 916080 の反応式
[C:1]([O:5][C:6](=[O:26])[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=1[CH2:13][S:14][C:15]1[NH:16][C:17]2[CH:23]=[C:22]([CH3:24])[C:21]([CH3:25])=[CH:20][C:18]=2[N:19]=1)([CH3:4])([CH3:3])[CH3:2].C(N(CC)CC)C.[C:34](Cl)(=[O:41])[C:35]1[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=1.O>C(Cl)(Cl)Cl>[C:1]([O:5][C:6](=[O:26])[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=1[CH2:13][S:14][C:15]1[N:16]([C:34]([C:35]2[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=2)=[O:41])[C:17]2[CH:23]=[C:22]([CH3:24])[C:21]([CH3:25])=[CH:20][C:18]=2[N:19]=1)([CH3:4])([CH3:3])[CH3:2]

参加物

6

反応物 4

HCID 962WaterHCID 7412Benzoyl chlorideHCID 8471TriethylamineHCID 694570282-((5,6-Dimethylbenzimidazole-2-ylthio)methyl)benzoic acid t-butyl ester

生成物 1

HCID 694582302-((5,6-Dimethyl-1-(phenylcarbonyl)benzimidazole-2-ylthio)methyl)benzoic acid t-butyl ester

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

2-((5,6-dimethylbenzimidazole-2-ylthio)methyl)benzoic acid t-butyl ester (30 mg, 0.082 mmol) was dissolved in 3 ml of chloroform, to which triethylamine (17 μl, 0.123 mmol) and benzoyl chloride (14 μl, 0.123 mmol) were sequentially added and the mixture was stirred at room temperature for 2 hours. After the reaction was complete, water was added, followed by extraction with ethyl acetate. After drying the ethyl acetate phase with anhydrous sodium sulfate, it was concentrated, and 2-((5,6-dimethyl-1-(phenylcarbonyl)benzimidazole-2-ylthio)methyl)benzoic acid t-butyl ester was obtained (38 mg, yield quantitative).

後処理

  1. additionwere sequentially added
  2. extractionfollowed by extraction with ethyl acetate
  3. dry with materialAfter drying the ethyl acetate phase with anhydrous sodium sulfate, it
  4. concentrationwas concentrated

出典と根拠

ORDレコード
ord-ad49f7b84bbc4d8d9dbf4150bf890d56
出典データセット
uspto-grants-2007_09
特許番号
US07268145B2

反応ノート

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