Diisopropylethylamine → 2-[2-[[4-[5-{2,8-Dimethyl-5H-dibenzo[a,d]cyclohepten-5-yl}-3,4-dihydro-2,4-dioxo-1(2H)-pyrimidinyl]pyrimidin-2-yl]amino]acetylamino]-4-thiazoleacetic acid, ethyl ester

HRID 1871976노트

반응식

HRID 1871976 반응식
[NH2:1][CH2:2][C:3]([NH:5][C:6]1[S:7][CH:8]=[C:9]([CH2:11][C:12]([O:14][CH2:15][CH3:16])=[O:13])[N:10]=1)=[O:4].C(N(CC)C(C)C)(C)C.Cl[C:27]1[N:32]=[C:31]([N:33]2[CH:38]=[C:37]([CH:39]3[C:45]4[CH:46]=[CH:47][C:48]([CH3:50])=[CH:49][C:44]=4[CH:43]=[CH:42][C:41]4[CH:51]=[C:52]([CH3:55])[CH:53]=[CH:54][C:40]3=4)[C:36](=[O:56])[NH:35][C:34]2=[O:57])[CH:30]=[CH:29][N:28]=1>CN1CCCC1=O>[CH3:50][C:48]1[CH:47]=[CH:46][C:45]2[CH:39]([C:37]3[C:36](=[O:56])[NH:35][C:34](=[O:57])[N:33]([C:31]4[CH:30]=[CH:29][N:28]=[C:27]([NH:1][CH2:2][C:3]([NH:5][C:6]5[S:7][CH:8]=[C:9]([CH2:11][C:12]([O:14][CH2:15][CH3:16])=[O:13])[N:10]=5)=[O:4])[N:32]=4)[CH:38]=3)[C:40]3[CH:54]=[CH:53][C:52]([CH3:55])=[CH:51][C:41]=3[CH:42]=[CH:43][C:44]=2[CH:49]=1

참가 물질

5

실험 절차

A mixture of the product from step (i) (0.194 g), N,N-diisopropylethylamine (0.35 ml) and the product from example 8 step (ii) (0.25 g) in 1-methyl-2-pyrrolidinone (5 ml) was heated at 90° C. for 10 hours. The mixture was partitioned between ethyl acetate and water. The organic phase was washed with water, dried (MgSO4) and evaporated. Purification was by chromatography eluting with 70% ethyl acetate in isohexane. Yield 0.175 g.

후처리

  1. customThe mixture was partitioned between ethyl acetate and water
  2. washThe organic phase was washed with water
  3. dry with materialdried (MgSO4)
  4. customevaporated
  5. customPurification
  6. washeluting with 70% ethyl acetate in isohexane

출처 및 근거

ORD 기록
ord-9c2517e308244bacbf297f5d9fd97b92
출처 데이터셋
uspto-grants-2000_08
특허 번호
US06107297

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