Amidinothiourea → HCID 178428480, 화합물

HRID 1059906

반응식

HRID 1059906 반응식
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]

참가 물질

4

반응물 2

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

생성물 1

HCID 178428480HCID 178428480, 화합물수율 74.7%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-9da09301d0ea4e07ab4d8449da8eb08b
출처 데이터셋
uspto-grants-2003_02
특허 번호
US06521643B1

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