Tetrahydrofuran → 4-Chloro-2-methanesulfonyl-thieno[2,3-d]pyrimidine-6-carboxylic acid methyl ester

HRID 1694849노트

반응식

HRID 1694849 반응식
[CH3:1][O:2][C:3]([C:5]1[S:16][C:8]2[N:9]=[C:10](SC)[N:11]=[C:12]([Cl:13])[C:7]=2[CH:6]=1)=[O:4].O[O:18][S:19]([O-:21])=O.[K+].[CH2:23]1COCC1>O>[CH3:1][O:2][C:3]([C:5]1[S:16][C:8]2[N:9]=[C:10]([S:19]([CH3:23])(=[O:21])=[O:18])[N:11]=[C:12]([Cl:13])[C:7]=2[CH:6]=1)=[O:4]

참가 물질

5

반응물 3

HCID 8028TetrahydrofuranHCID 23707502Potassium hydroxy sulfiteHCID 59376433Methyl 4-chloro-2-(methylthio)thieno[2,3-d]pyrimidine-6-carboxylate

생성물 1

HCID 593764254-Chloro-2-methanesulfonyl-thieno[2,3-d]pyrimidine-6-carboxylic acid methyl ester

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a solution of 4-chloro-2-methylsulfanyl-thieno[2,3-d]pyrimidine-6-carboxylic acid methyl ester (3.3 g, 12.0 mmol) in THF (150 mL) was added a solution of Oxone (15.5 g, 25.2 mmol) in H2O (80 mL) dropwise at RT. After 18 h, the solvent was removed and the residue was diluted with CH2Cl2. The organic fraction was washed with water (1×), brine (1×), dried over. MgSO4, and concentrated. The residue was used without further purification. ESIMS calcd 307 (M++H), found 307 (M++H).

후처리

  1. customthe solvent was removed
  2. additionthe residue was diluted with CH2Cl2
  3. washThe organic fraction was washed with water (1×), brine (1×)
  4. customdried over
  5. concentrationMgSO4, and concentrated
  6. customThe residue was used without further purification

출처 및 근거

ORD 기록
ord-460bc04865d84d25a1ae69489b648e27
출처 데이터셋
uspto-grants-2012_04
특허 번호
US08158825B2

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