Sodium Bicarbonate → HCID 69218334, 화합물

HRID 2251082노트

반응식

HRID 2251082 반응식
[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]

참가 물질

7

반응물 4

HCID 516892Sodium BicarbonateHCID 10313463Potassium peroxymonosulphateHCID 23707502Potassium hydroxy sulfiteHCID 69218825HCID 69218825, 화합물

생성물 1

HCID 69218334HCID 69218334, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 21899815MeOH tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-07d4e6a3af7b445794844495e44ab6f3
출처 데이터셋
uspto-grants-2008_01
특허 번호
US07319102B1

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