Methylamine → HCID 86756619, 화합물

HRID 324495노트

반응식

HRID 324495 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][NH2:27]>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]([NH:27][CH3:26])[S:3][C:4]=3[CH:11]=[CH:10][C:9]=2[CH:12]=1

참가 물질

4

반응물 2

HCID 6329MethylamineHCID 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 86756619HCID 86756619, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

The product from example 44 step (viii) (0.05 g) was heated with 40% aq. Methylamine (4 ml) in ethanol (1 ml) for 3 hours. 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/iso-hexane 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/iso-hexane mixtures
  6. filtrationthe title product collected by filtration as a pale yellow solid

출처 및 근거

ORD 기록
ord-704be0583aca46c18803d136c4229b03
출처 데이터셋
uspto-grants-2001_04
특허 번호
US06218376B1

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