Sodium Sulfite → 3,8-Difluoro-4-hydroxy-4-(hydroxymethyl)-4,5-dihydro-7H-pyrrolo[3,2,1-de]-1,5-naphthyridin-7-one

HRID 15137

반응식

HRID 15137 반응식
[F:1][C:2]1[CH:3]=[N:4][C:5]2[CH:6]=[C:7]([F:16])[C:8](=[O:15])[N:9]3CC(=C)C=1[C:10]=23.S([O-])([O-])=O.[Na+].[Na+].[C:23]([OH:27])([CH3:26])([CH3:25])[CH3:24].[OH2:28]>>[F:1][C:2]1[CH:3]=[N:4][C:5]2[CH:6]=[C:7]([F:16])[C:8](=[O:15])[N:9]3[CH2:25][C:23]([OH:27])([CH2:26][OH:28])[C:24]=1[C:10]=23

참가 물질

4

실험 절차

A solution of 3,8-difluoro-4-methylidene-4,5-dihydro-7H-pyrrolo[3,2,1-de]-1,5-naphthyridin-7-one (631 mg, 2.9 mmol) in tert-butanol/water (30 ml/30 ml) was treated with AD mix alpha (4.3 g) under argon. After 18 hours stirring the reaction mixture was treated with saturated sodium sulphite solution (30 ml). After 10 minutes stirring the mixture was extracted with 20% methanol in dichloromethane (3×300 ml). The organic extracts were dried over magnesium sulphate and evaporated affording a white solid (710 mg, 97%).

후처리

  1. additionmix alpha (4.3 g) under argon
  2. stirringAfter 10 minutes stirring the mixture
  3. extractionwas extracted with 20% methanol in dichloromethane (3×300 ml)
  4. dry with materialThe organic extracts were dried over magnesium sulphate
  5. customevaporated

출처 및 근거

ORD 기록
ord-c9aded2d0f824bf9b94d7c7d4dcc8f67
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07732460B2

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