Carbon Disulfide → (2-{[(5-Methyl-1H-imidazol-4-yl)methyl]sulfanyl}ethyl)carbamodithioic acid

HRID 372268

반응식

HRID 372268 반응식
[CH3:1][C:2]1[NH:6][CH:5]=[N:4][C:3]=1[CH2:7][S:8][CH2:9][CH2:10][NH2:11].[C:12](=[S:14])=[S:13]>C(O)C>[CH3:1][C:2]1[NH:6][CH:5]=[N:4][C:3]=1[CH2:7][S:8][CH2:9][CH2:10][NH:11][C:12](=[S:13])[SH:14]

참가 물질

4

반응물 2

HCID 6348Carbon DisulfideHCID 6655684-(((2-Aminoethyl)thio)methyl)-5-methylimidazole

생성물 1

HCID 15566013(2-{[(5-Methyl-1H-imidazol-4-yl)methyl]sulfanyl}ethyl)carbamodithioic acid

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A solution of 2-((5-methyl-4-imidazolyl)methylthio)ethylamine (10.2 g) in ethanol (75 ml) was added slowly, with stirring, to carbon disulphide (200 ml). The mixture was set aside overnight at room temperature and the solid formed was collected and recrystallised from aqueous isopropyl alcohol to afford N-[2-((5-methyl-4-imidazolyl)methylthio)ethyl]dithiocarbamic acid (9.8 g), m.p. 127°-129°. This was treated with dicyclohexylcarbodiimide in dry pyridine at -10°, and the mixture was filtered. The filtrate was evaporated to dryness and the residue was treated sith ethanolic hydrogen chloride to give 5-methyl-4-(2-isothiocyanatoethylthiomethyl)imidazole hydrochloride.

후처리

  1. customthe solid formed
  2. customwas collected
  3. customrecrystallised from aqueous isopropyl alcohol

출처 및 근거

ORD 기록
ord-d1d9af87a0e9408d9417ba1c529e7d42
출처 데이터셋
uspto-grants-1978_05
특허 번호
US04090026

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