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

HRID 439301ノート

反応式

HRID 439301 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e50cfb74c4cd4ca6b45e05c723e1a1f7
出典データセット
uspto-grants-1996_05
特許番号
US05514643

反応ノート

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