2-(chloromethyl)-N,N-dimethylaniline hydrochloride → 4-(2-Dimethylaminobenzylthio)-5,5-dimethyl-3-imidazolin-2-one

HRID 3241노트

반응식

HRID 3241 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.[CH3:13][C:14]1([CH3:21])[NH:18][C:17](=[O:19])[NH:16][C:15]1=[S:20]>CO>[CH3:2][N:3]([CH3:12])[C:4]1[CH:11]=[CH:10][CH:9]=[CH:8][C:5]=1[CH2:6][S:20][C:15]1[C:14]([CH3:21])([CH3:13])[NH:18][C:17](=[O:19])[N:16]=1

참가 물질

4

반응물 2

HCID 135374262-(chloromethyl)-N,N-dimethylaniline hydrochlorideHCID 189348924,4-Dimethyl-5-sulfanylideneimidazolidin-2-one

생성물 1

HCID 189348884-(2-Dimethylaminobenzylthio)-5,5-dimethyl-3-imidazolin-2-one

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Initially, 2.5 g of 2-dimethylaminobenzylchloride hydrochloride was added to a solution of 1.5 g of 5,5-dimethyl-4-thiohydantoin in 50 mL of methanol (MeQH). The reaction mixture was stirred for two hours at the room temperature and concentrated in vacuo. To the residue, there was added 100 mL of CHCl3. The residue was washed two times with 100 mL of aqueous solution of NaHCO3, dried over MgSO4 and concentrated in vacuo. The residue purified by column chromatography [CHCl3 :MeOH=100:1 (v/v)]. Recrystallized from diethyl ether gave the desired compound in the form of needle-like crystal. The yield of this compound was 2 g with a yield ratio of 69.1%, and the melting point was 160°-162° C.

후처리

  1. concentrationconcentrated in vacuo
  2. additionTo the residue, there was added 100 mL of CHCl3
  3. washThe residue was washed two times with 100 mL of aqueous solution of NaHCO3
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated in vacuo
  6. customThe residue purified by column chromatography [CHCl3 :MeOH=100:1 (v/v)]
  7. customRecrystallized from diethyl ether

출처 및 근거

ORD 기록
ord-673e7e0da0374e52b0efea0bb7e74951
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05733922

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