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

HRID 324496ノート

反応式

HRID 324496 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][NH:27][CH3:28]>C(O)C>[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]([N:27]([CH3:28])[CH3:26])[S:3][C:4]=3[CH:11]=[CH:10][C:9]=2[CH:12]=1

参加物

4

反応物 2

HCID 674DimethylamineHCID 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 70113722(+/-)-5-(7-Chloro-2-dimethylamino-4H-benzo[5,6]cyclohepta[1,2-d]thiazol-4-yl)-1-methyl-2,4(1H,3H)-pyrimidinedione

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

The product from example 44 step (viii) (0.05 g) was heated with 40% aq. dimethylamine (2 ml) in ethanol (1 ml) for 1 hour. The mixture was partitioned between ethyl acetate and water. The organic phase was collected, dried (MgSO4) and solvent evaporated under reduced pressure. The residue was triturated with ethyl acetate/isohexane mixtures and the title product collected by filtration as a pale yellow solid.

後処理

  1. customThe mixture was partitioned between ethyl acetate and water
  2. customThe organic phase was collected
  3. dry with materialdried (MgSO4) and solvent
  4. customevaporated under reduced pressure
  5. customThe residue was triturated with ethyl acetate/isohexane mixtures
  6. filtrationthe title product collected by filtration as a pale yellow solid

出典と根拠

ORDレコード
ord-f7b1c4489fe34e21bbc6312f5fb6c4d0
出典データセット
uspto-grants-2001_04
特許番号
US06218376B1

反応ノート

読み込み中…