3-(Diethylamino)propyl isothiocyanate → N'-[3-(Diethylamino)propyl]-N-(1-methylethyl)-N-[2-(phenylsulfonyl)ethyl]thiourea

HRID 745186

반응식

HRID 745186 반응식
[C:1]1([S:7]([CH2:10][CH2:11][NH:12][CH:13]([CH3:15])[CH3:14])(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH2:16]([N:18]([CH2:21][CH2:22][CH2:23][N:24]=[C:25]=[S:26])[CH2:19][CH3:20])[CH3:17]>C(#N)C>[CH2:19]([N:18]([CH2:16][CH3:17])[CH2:21][CH2:22][CH2:23][NH:24][C:25](=[S:26])[N:12]([CH:13]([CH3:15])[CH3:14])[CH2:11][CH2:10][S:7]([C:1]1[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1)(=[O:8])=[O:9])[CH3:20]

참가 물질

4

반응물 2

HCID 27582403-(Diethylamino)propyl isothiocyanateHCID 13655034N-(2-phenylsulfonylethyl)-2-propanamine

생성물 1

HCID 13655152N'-[3-(Diethylamino)propyl]-N-(1-methylethyl)-N-[2-(phenylsulfonyl)ethyl]thiourea수율 76.9%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A solution of 5.0 g (0.022 mole) of N-[2-(phenylsulfonyl)ethyl]-2-propanamine and 4.30 g (0.025 mole) of 3-(N,N-diethylamino)propylisothiocyanate in 400 ml of acetonitrile was refluxed for 16 hr. The solvent was removed in vacuo and the residue was dissolved in ether. The solution was extracted with three portions of water and was dried over magnesium sulfate. The volume of the ether solution was reduced to 200 ml, and hexane was added until the solution became slightly cloudy. A white solid precipitated to give 6.76 g (76.9%) of white crystalline solid, m.p. 120°-121° C.

후처리

  1. customThe solvent was removed in vacuo
  2. dissolutionthe residue was dissolved in ether
  3. extractionThe solution was extracted with three portions of water
  4. dry with materialwas dried over magnesium sulfate
  5. additionwas added until the solution
  6. customA white solid precipitated

출처 및 근거

ORD 기록
ord-91a18e96e5dc466494837ac45fa13f6b
출처 데이터셋
uspto-grants-1986_07
특허 번호
US04597902

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