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HCID 20677558, 화합물 → HCID 23512569, 화합물

HRID 650639
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HRID 650639 반응식
C(O[C:6](=O)[N:7](C)[C:8]1[C:9]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=2[CH3:22])=[N:10][C:11]([S:14][CH3:15])=[N:12][CH:13]=1)(C)(C)C>CO.Cl>[CH3:6][NH:7][C:8]1[C:9]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=2[CH3:22])=[N:10][C:11]([S:14][CH3:15])=[N:12][CH:13]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 1

HCID 20677558HCID 20677558, 화합물

생성물 1

HCID 23512569HCID 23512569, 화합물수율 94%

시약·촉매·용매 1

HCID 21893726Hydrochloride methanol용매

실험 절차

A solution of 1.95 g (5.64 mmol) methyl-(2-methylsulfanyl-4-o-tolyl-pyrimidin-5-yl)-carbamic acid tert-butyl ester in 30 ml MeOH/HCl (2N) was stirred at 50° for 3 hr. After evaporation of the solvent, the residue was distributed between 40 ml 1N NaOH and 40 ml CH2Cl2. The phases were separated, the aqueous layer washed twice with 50 ml CH2Cl2. The combined organic layers were dried (Na2SO4), filtered and evaporated. The residue was purified by chromatography (SiO2, CH2Cl2/ethyl acetate 10:1) to give 1.30 g (94%) methyl-(2-methylsulfanyl-4-o-tolyl-pyrimidin-5-yl)-amine as a white solid, MS (EI): 245 (M+).

후처리

  1. customAfter evaporation of the solvent
  • customThe phases were separated
  • washthe aqueous layer washed twice with 50 ml CH2Cl2
  • dry with materialThe combined organic layers were dried (Na2SO4)
  • filtrationfiltered
  • customevaporated
  • customThe residue was purified by chromatography (SiO2, CH2Cl2/ethyl acetate 10:1)
  • 출처 및 근거

    ORD 기록
    ord-06d2e0e3bca34922aad47c92413c944e
    출처 데이터셋
    uspto-grants-2001_08
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US06274588B1

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