Sodium Methoxide → (+/-)-5-(7-Chloro-2-methoxy-4H-benzo[5,6]cyclohepta[1,2-d]thiazol-4-yl)-1-methyl-2,4(1H,3H)-pyrimidinedione

HRID 324493노트

반응식

HRID 324493 반응식
Cl[C:2]1[S:3][C:4]2[CH:11]=[CH:10][C:9]3[CH:12]=[C:13]([Cl:16])[CH:14]=[CH:15][C:8]=3[CH:7]([C:17]3[C:18](=[O:25])[NH:19][C:20](=[O:24])[N:21]([CH3:23])[CH:22]=3)[C:5]=2[N:6]=1.[CH3:26][O-:27].[Na+]>>[Cl:16][C:13]1[CH:14]=[CH:15][C:8]2[CH:7]([C:17]3[C:18](=[O:25])[NH:19][C:20](=[O:24])[N:21]([CH3:23])[CH:22]=3)[C:5]3[N:6]=[C:2]([O:27][CH3:26])[S:3][C:4]=3[CH:11]=[CH:10][C:9]=2[CH:12]=1

참가 물질

3

반응물 2

HCID 10942334Sodium MethoxideHCID 70113243(+/-)-5-(2,7-Dichloro-4H-benzo[5,6]cyclohepta[1,2-d]thiazol-4-yl)-1-methyl-2,4(1H,3H)-pyrimidinedione

생성물 1

HCID 70112888(+/-)-5-(7-Chloro-2-methoxy-4H-benzo[5,6]cyclohepta[1,2-d]thiazol-4-yl)-1-methyl-2,4(1H,3H)-pyrimidinedione

실험 절차

The product from example 44 step (viii) (0.1 g) was heated with a solution of sodium methoxide (made from sodium (0.2 g) in dry methanol (10 ml)) at reflux for 3 h. The mixture was partitioned between ethyl acetate and water. The organic phase was collected, dried (MgSO4) and solvent evaporated under reduced pressure. Purification was by chromatography eluting with 70% ethyl acetate in isohexane to give the title product as a colourless solid.

후처리

  1. temperatureat reflux for 3 h
  2. customThe mixture was partitioned between ethyl acetate and water
  3. customThe organic phase was collected
  4. dry with materialdried (MgSO4) and solvent
  5. customevaporated under reduced pressure
  6. customPurification
  7. washeluting with 70% ethyl acetate in isohexane

출처 및 근거

ORD 기록
ord-21bdb3aea67b4e769618dc153de41058
출처 데이터셋
uspto-grants-2001_04
특허 번호
US06218376B1

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