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

HRID 1694849ノート

反応式

HRID 1694849 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-460bc04865d84d25a1ae69489b648e27
出典データセット
uspto-grants-2012_04
特許番号
US08158825B2

反応ノート

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