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

HRID 3252노트

반응식

HRID 3252 반응식
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

참가 물질

4

반응물 2

HCID 135374262-(chloromethyl)-N,N-dimethylaniline hydrochlorideHCID 178418227HCID 178418227, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-9a24f90cc7884da083a28d124bc01ed8
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05733922

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