Sodium Bicarbonate → HCID 69218334、化合物

HRID 2251082ノート

反応式

HRID 2251082 の反応式
[CH2:1]([O:3][C:4](=[O:33])[CH:5]=[C:6]([C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][C:27]=1[Cl:32])[C:7]1[N:17]([C:18]2[C:23]([F:24])=[CH:22][CH:21]=[CH:20][C:19]=2[F:25])[C:10]2[N:11]=[C:12](SC)[N:13]=[CH:14][C:9]=2[CH:8]=1)[CH3:2].O[O:35][S:36]([O-:38])=O.[K+].S([O-])(O[O-])(=O)=O.[K+].[K+].[C:48]([O-])(O)=O.[Na+]>C1COCC1.CO.O>[CH2:1]([O:3][C:4](=[O:33])[CH:5]=[C:6]([C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][C:27]=1[Cl:32])[C:7]1[N:17]([C:18]2[C:23]([F:24])=[CH:22][CH:21]=[CH:20][C:19]=2[F:25])[C:10]2[N:11]=[C:12]([S:36]([CH3:48])(=[O:38])=[O:35])[N:13]=[CH:14][C:9]=2[CH:8]=1)[CH3:2]

参加物

7

反応物 4

HCID 516892Sodium BicarbonateHCID 10313463Potassium peroxymonosulphateHCID 23707502Potassium hydroxy sulfiteHCID 69218825HCID 69218825、化合物

生成物 1

HCID 69218334HCID 69218334、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 21899815MeOH tetrahydrofuran溶媒

実験手順

To a solution of 3-(2-chloro-phenyl)-3-[7-(2,6-difluorophenyl)-2-methylsulfanyl-7H-pyrrolo[2,3-d]pyrimidin-6-yl]-acrylic acid ethyl ester, 13, (0.33 g, 0.68 mmol) in THF/methanol (4 mL of 1:1 mixture) is added dropwise a solution of Oxone® (potassium peroxymonosulfate) (1.46 g, 2.38 mmol) in H2O (4 mL). After stirring the reaction for 1 hour at room temperature, the solution is poured into aqueous saturated NaHCO3. The aqueous phase is extracted with CHCl3 and the combined organic phases are dried (MgSO4), filtered and concentrated in vacuo to afford 0.31 g of the desired product which is used without further purification.

後処理

  1. customthe reaction for 1 hour at room temperature
  2. extractionThe aqueous phase is extracted with CHCl3
  3. dry with materialthe combined organic phases are dried (MgSO4)
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-07d4e6a3af7b445794844495e44ab6f3
出典データセット
uspto-grants-2008_01
特許番号
US07319102B1

反応ノート

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