Amidinothiourea → HCID 178428480、化合物

HRID 1059906

反応式

HRID 1059906 の反応式
Cl[CH:2]([CH3:12])[C:3]([C:5]1[CH:10]=[C:9]([CH3:11])[CH:8]=[CH:7][N:6]=1)=O.[C:13]([NH2:19])([NH2:18])=[N:14][C:15]([NH2:17])=[S:16]>C(O)C>[NH:14]([C:15]1[S:16][C:2]([CH3:12])=[C:3]([C:5]2[CH:10]=[C:9]([CH3:11])[CH:8]=[CH:7][N:6]=2)[N:17]=1)[C:13]([NH2:19])=[NH:18]

参加物

4

反応物 2

HCID 2724563AmidinothioureaHCID 186674842-Chloro-1-(4-methylpyridin-2-yl)propan-1-one

生成物 1

HCID 178428480HCID 178428480、化合物収率 74.7%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution of 2-chloro-1-(4-methylpyridin-2-yl)propan-1-one (0.4 g) in ethanol (5 ml) was added 2-imino-4-thiobiuret (257 mg). The mixture was refluxed for 2 hours, and the solvent was evaporated under reduced pressure. To the residue were added ethyl acetate and a saturated aqueous sodium hydrogencarbonate solution. The ethyl acetate layer was separated, washed with brine, dried over sodium sulfate and evaporated under reduced pressure. The residue was purified by column chromatography (silica gel 25 g, dichloromethane:methanol:triethylamine=80:10:1) to give 2-guanidino-5-methyl-4-(4-methylpyridin-2-yl)thiazole (402 mg).

後処理

  1. temperatureThe mixture was refluxed for 2 hours
  2. customthe solvent was evaporated under reduced pressure
  3. additionTo the residue were added ethyl acetate
  4. customThe ethyl acetate layer was separated
  5. washwashed with brine
  6. dry with materialdried over sodium sulfate
  7. customevaporated under reduced pressure
  8. customThe residue was purified by column chromatography (silica gel 25 g, dichloromethane:methanol:triethylamine=80:10:1)

出典と根拠

ORDレコード
ord-9da09301d0ea4e07ab4d8449da8eb08b
出典データセット
uspto-grants-2003_02
特許番号
US06521643B1

関連ノート

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