But-2-yn-1-amine → HCID 178449099, 화합물

HRID 27381

반응식

HRID 27381 반응식
[N+:1]([CH:4]=[C:5](SC)[NH:6][CH2:7][CH2:8][S:9][CH2:10][C:11]1[NH:15][CH:14]=[N:13][C:12]=1[CH3:16])([O-:3])=[O:2].[CH2:19]([NH2:23])[C:20]#[C:21][CH3:22]>C(#N)C>[N+:1]([CH:4]=[C:5]([NH:23][CH2:19][C:20]#[C:21][CH3:22])[NH:6][CH2:7][CH2:8][S:9][CH2:10][C:11]1[NH:15][CH:14]=[N:13][C:12]=1[CH3:16])([O-:3])=[O:2]

참가 물질

4

반응물 2

HCID 12599998But-2-yn-1-amineHCID 178503826HCID 178503826, 화합물

생성물 1

HCID 178449099HCID 178449099, 화합물수율 80%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A mixture of 1-nitro-2-methylthio-2-{2-[(4-methyl-1H-imidazol-5-yl)methylthio]ethylamino}ethylene (2.25 g, 7.8 mmole) and 2-butyn-1-amine (2.16 g, 31.2 mmole) in acetonitrile (35 ml) was stirred under a positive pressure of nitrogen at reflux temperature for 7 hours and at room temperature for 15 hours. The solvent was removed by evaporation under reduced pressure, and the residue placed on silica gel and chromatographed by gradient elution using methylene chloride-methanol. The appropriate fractions yielded 1.93 g (80%) of the title product from acetonitrile. Recrystallization from isopropyl alcohol gave the product with mp 147.5°-151°.

후처리

  1. temperatureat reflux temperature for 7 hours
  2. customThe solvent was removed by evaporation under reduced pressure
  3. customchromatographed by gradient elution

출처 및 근거

ORD 기록
ord-cb5192f8f86244b28cb277a0844b27e9
출처 데이터셋
uspto-grants-1980_09
특허 번호
US04221737

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