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 324496노트

반응식

HRID 324496 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][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

참가 물질

4

반응물 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

생성물 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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f7b1c4489fe34e21bbc6312f5fb6c4d0
출처 데이터셋
uspto-grants-2001_04
특허 번호
US06218376B1

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