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 324493ノート

反応式

HRID 324493 の反応式
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

参加物

3

反応物 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

生成物 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

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-21bdb3aea67b4e769618dc153de41058
出典データセット
uspto-grants-2001_04
特許番号
US06218376B1

反応ノート

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