2-(chloromethyl)-N,N-dimethylaniline hydrochloride → 2-benzylthio-4-(2-dimethylaminobenzylthio)-5,5-dimethyl-5H-imidazole

HRID 3252ノート

反応式

HRID 3252 の反応式
Cl.[CH3:2][N:3]([CH3:12])[C:4]1[CH:11]=[CH:10][CH:9]=[CH:8][C:5]=1[CH2:6]Cl.[CH2:13]([S:20][C:21]1[NH:22][C:23]([CH3:28])([CH3:27])[C:24](=[S:26])[N:25]=1)[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1>C(O)C>[CH2:13]([S:20][C:21]1[N:25]=[C:24]([S:26][CH2:6][C:5]2[CH:8]=[CH:9][CH:10]=[CH:11][C:4]=2[N:3]([CH3:12])[CH3:2])[C:23]([CH3:28])([CH3:27])[N:22]=1)[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1

参加物

4

反応物 2

HCID 135374262-(chloromethyl)-N,N-dimethylaniline hydrochlorideHCID 178418227HCID 178418227、化合物

生成物 1

HCID 189348372-benzylthio-4-(2-dimethylaminobenzylthio)-5,5-dimethyl-5H-imidazole

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Initially, 0.65 g of 2-dimethylaminobenzylchloride hydrochloride was added to a solution of 0.7 g of 2-benzylthio-5,5-dimethylimidazolin-4-thione in 20 mL of ethanol (EtOH). The reaction mixture was stirred at the room temperature for one hour, and concentrated in vacuo. The residue was treated following the procedure used in Example 62, and purified by column chromatography (CHCl3). Recrystallization from diethyl ether-n-hexane gave 2-benzylthio-4-(2-dimethylaminobenzylthio)-5,5-dimethyl-5H-imidazole in the form of a needle-like crystal. The yield of this compound was 0.75 g with a yield ratio of 72.2%, and the melting point was 91°-92° C.

後処理

  1. concentrationconcentrated in vacuo
  2. additionThe residue was treated
  3. custompurified by column chromatography (CHCl3)
  4. customRecrystallization from diethyl ether-n-hexane

出典と根拠

ORDレコード
ord-9a24f90cc7884da083a28d124bc01ed8
出典データセット
uspto-grants-1998_03
特許番号
US05733922

反応ノート

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