Sodium Sulfite → Tert-butyl 2-(methylsulfonyl)-5H-pyrrolo[3,4-D]pyrimidine-6(7H)-carboxylate

HRID 459493노트

반응식

HRID 459493 반응식
Cl[C:2]1C=CC=C(C(OO)=O)C=1.[C:12]([O:16][C:17]([N:19]1[CH2:27][C:26]2[CH:25]=[N:24][C:23](SC)=[N:22][C:21]=2[CH2:20]1)=[O:18])([CH3:15])([CH3:14])[CH3:13].[S:30]([O-:33])([O-])=[O:31].[Na+].[Na+].C(=O)([O-])O.[Na+]>ClCCl>[C:12]([O:16][C:17]([N:19]1[CH2:27][C:26]2[CH:25]=[N:24][C:23]([S:30]([CH3:2])(=[O:33])=[O:31])=[N:22][C:21]=2[CH2:20]1)=[O:18])([CH3:15])([CH3:13])[CH3:14]

참가 물질

6

반응물 4

HCID 24437Sodium SulfiteHCID 70297m-Chloroperbenzoic acidHCID 516892Sodium BicarbonateHCID 18442822Tert-butyl 2-(methylthio)-5H-pyrrolo[3,4-D]pyrimidine-6(7H)-carboxylate

생성물 1

HCID 18442821Tert-butyl 2-(methylsulfonyl)-5H-pyrrolo[3,4-D]pyrimidine-6(7H)-carboxylate

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

m-Chloroperbenzoic acid (1.99 g) was added to a dichloromethane solution (20 ml) of 6-(tert-butoxy-carbonyl)-5,7-dihydro-2-methylthiopyrrolo[3,4-d]-pyrimidine (1.08 g) under ice cooling, and the mixture was stirred for 5 hours. A saturated aqueous solution of sodium sulfite, a saturated aqueous solution of sodium hydrogen carbonate and dichloromethane were added to separate an organic layer. The organic layer was then dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure, hexane was added to the residue, and powder deposited was collected by filtration to obtain the title compound (1.09 g) as colorless powder.

후처리

  1. customto separate an organic layer
  2. dry with materialThe organic layer was then dried over anhydrous sodium sulfate
  3. distillationThe solvent was distilled off under reduced pressure, hexane
  4. additionwas added to the residue, and powder
  5. filtrationdeposited was collected by filtration

출처 및 근거

ORD 기록
ord-818e0be7aab842d1bbbc956bfd221c01
출처 데이터셋
uspto-grants-2007_03
특허 번호
US07192968B2

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