Hydrogen Sulfide → 2-Cyclopropylamino-4-methyl-thiazole-5-carboxylic acid (thiocarbamoyl-thiophen-2-yl-methyl)-amide

HRID 439301노트

반응식

HRID 439301 반응식
[C:1]([CH:3]([NH:9][C:10]([C:12]1[S:16][C:15]([NH:17][CH:18]2[CH2:20][CH2:19]2)=[N:14][C:13]=1[CH3:21])=[O:11])[C:4]1[S:5][CH:6]=[CH:7][CH:8]=1)#[N:2].C(N(CC)CC)C.[SH2:29]>C(O)C>[C:1]([CH:3]([NH:9][C:10]([C:12]1[S:16][C:15]([NH:17][CH:18]2[CH2:20][CH2:19]2)=[N:14][C:13]=1[CH3:21])=[O:11])[C:4]1[S:5][CH:6]=[CH:7][CH:8]=1)(=[S:29])[NH2:2]

참가 물질

5

반응물 3

HCID 402Hydrogen SulfideHCID 8471TriethylamineHCID 543672022-Cyclopropylamino-4-methyl-thiazole-5-carboxylic acid (cyano-thiophen-2-yl-methyl)-amide

생성물 1

HCID 543298972-Cyclopropylamino-4-methyl-thiazole-5-carboxylic acid (thiocarbamoyl-thiophen-2-yl-methyl)-amide수율 88%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

0.72g of 2-cyclopropylamino-4-methyl-thiazole-5-carboxylic acid (cyano-thiophen-2-yl-methyl)-amide (12) was dissolved in 10ml of ethanol and then 0.63ml of triethylamine was added thereto. The reaction solution was stirred under reflux for 8 hours while introducing hydrogen sulfide gas. After removing the solvent, water was added to the residue and then the solid product which is not dissolved in water was filtered. The filtered solid product was washed with diethylether and then dried to obtain 0.70g (Yield 88%) of the title compound.

후처리

  1. temperatureunder reflux for 8 hours
  2. customAfter removing the solvent, water
  3. additionwas added to the residue
  4. dissolutionthe solid product which is not dissolved in water
  5. filtrationwas filtered
  6. washThe filtered solid product was washed with diethylether
  7. customdried

출처 및 근거

ORD 기록
ord-e50cfb74c4cd4ca6b45e05c723e1a1f7
출처 데이터셋
uspto-grants-1996_05
특허 번호
US05514643

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