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HCID 20677558、化合物 → HCID 23512569、化合物

HRID 650639
ノート
印刷プレビュー

反応式

HRID 650639 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 1

HCID 20677558HCID 20677558、化合物

生成物 1

HCID 23512569HCID 23512569、化合物収率 94%

試薬・触媒・溶媒 1

HCID 21893726Hydrochloride methanol溶媒

実験手順

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+).

後処理

  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)
  • 出典と根拠

    ORDレコード
    ord-06d2e0e3bca34922aad47c92413c944e
    出典データセット
    uspto-grants-2001_08
    DOI
    10.6084/m9.figshare.5104873.v1
    特許番号
    US06274588B1

    反応ノート

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