반응식
Cl[CH2:2][C:3]([NH:5][C:6]1[CH:11]=[CH:10][C:9]([C:12]([N:14]2[C:20]3[CH:21]=[CH:22][CH:23]=[CH:24][C:19]=3[CH2:18][N:17]3[CH:25]=[CH:26][CH:27]=[C:16]3[CH2:15]2)=[O:13])=[CH:8][CH:7]=1)=[O:4].[NH:28]1[CH2:33][CH2:32][O:31][CH2:30][CH2:29]1.CN1CCCN(C)C1=O>C(Cl)Cl>[CH:27]1[CH:26]=[CH:25][N:17]2[CH2:18][C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=3[N:14]([C:12]([C:9]3[CH:10]=[CH:11][C:6]([NH:5][C:3](=[O:4])[CH2:2][N:28]4[CH2:33][CH2:32][O:31][CH2:30][CH2:29]4)=[CH:7][CH:8]=3)=[O:13])[CH2:15][C:16]=12참가 물질
반응물 3
생성물 1
시약·촉매·용매 1
실험 절차
A stirred suspension of 0.19 g of 2-chloro-N-[4-(5H-pyrrolo[2,1-c][1,4]benzodiazepin-10(11H)-ylcarbonyl)phenyl]acetamide in 1 ml of methylene chloride is added 0.44 g of morpholine followed by 1 ml of 1,3-di-methyl-3,4,5,6-tetrahydro-2(1H)-pyrimidinone and stirring continued for 20 hours. The methylene chloride is evaporated and the residue diluted with water. The resulting suspension is filtered and the precipitate washed with water. The brown solid is dissolved in 15 ml of ethyl acetate and washed with saturated NaHCO3, brine and dried with Na2SO4. The mixture is filtered and the filtrate evaporated in vacuo to give 0.23 g of a colorless gum which is stirred with ethyl acetate-hexanes to give 0.21 g of white solid. MS(CI): 431(M+H).
후처리
- customThe methylene chloride is evaporated
- additionthe residue diluted with water
- filtrationThe resulting suspension is filtered
- washthe precipitate washed with water
- dissolutionThe brown solid is dissolved in 15 ml of ethyl acetate
- washwashed with saturated NaHCO3, brine
- dry with materialdried with Na2SO4
- filtrationThe mixture is filtered
- customthe filtrate evaporated in vacuo
출처 및 근거
- ORD 기록
- ord-b58a69d7ccb643e6b7543dcded01e2ce
- 출처 데이터셋
- uspto-grants-1998_03
- 특허 번호
- US05733905
연결된 노트
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