Water → N-[4-(Pyrido[2,3-b][1,5]benzoxazepin-6(5H)-ylcarbonyl)-3-chlorophenyl][1,1'-biphenyl]-2-carboxamide

HRID 1457694

반응식

HRID 1457694 반응식
[N:1]1[C:6]2[O:7][C:8]3[CH:15]=[CH:14][CH:13]=[CH:12][C:9]=3[NH:10][CH2:11][C:5]=2[CH:4]=[CH:3][CH:2]=1.C(N(CC)C(C)C)(C)C.[C:25]1([C:44]2[CH:49]=[CH:48][CH:47]=[CH:46][CH:45]=2)[C:26]([C:31]([NH:33][C:34]2[CH:42]=[CH:41][C:37]([C:38](Cl)=[O:39])=[C:36]([Cl:43])[CH:35]=2)=[O:32])=[CH:27][CH:28]=[CH:29][CH:30]=1.O>ClCCl>[N:1]1[C:6]2[O:7][C:8]3[CH:15]=[CH:14][CH:13]=[CH:12][C:9]=3[N:10]([C:38]([C:37]3[CH:41]=[CH:42][C:34]([NH:33][C:31]([C:26]4[C:25]([C:44]5[CH:49]=[CH:48][CH:47]=[CH:46][CH:45]=5)=[CH:30][CH:29]=[CH:28][CH:27]=4)=[O:32])=[CH:35][C:36]=3[Cl:43])=[O:39])[CH2:11][C:5]=2[CH:4]=[CH:3][CH:2]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 81531DiisopropylethylamineHCID 158959295,6-Dihydropyrido[2,3-b][1,5]benzoxazepineHCID 220996004-[([1,1'-Biphenyl]-2-carbonyl)amino]-2-chlorobenzoyl chloride

생성물 1

HCID 22099925N-[4-(Pyrido[2,3-b][1,5]benzoxazepin-6(5H)-ylcarbonyl)-3-chlorophenyl][1,1'-biphenyl]-2-carboxamide

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A mixture of 0.198 g of 5,6-dihydropyrido[2,3-b][1,5]benzoxazepine, 0.155 g of N,N-diisopropylethylamine and 0.444 g of 4-[([1,1-biphenyl]-2-carbonyl)amino]-2-chlorobenzoyl chloride in 12 ml of dichloromethane is stirred at room temperature for 2.5 hours. The mixture is poured into water and extracted with dichloromethane. The extract is washed with 2N Na2CO3, H2O, brine and dried (Na2 SO4). The solution is passed through a thin pad of hydrous magnesium silicate. The filter pad is washed with 50 ml of hexane-ethyl acetate (1:2) and the filtrate concentrated to dryness.

후처리

  1. extractionextracted with dichloromethane
  2. washThe extract is washed with 2N Na2CO3, H2O, brine
  3. customdried (Na2 SO4)
  4. washThe filter pad is washed with 50 ml of hexane-ethyl acetate (1:2)
  5. concentrationthe filtrate concentrated to dryness

출처 및 근거

ORD 기록
ord-fe7620382d5a4248a662034564e8e059
출처 데이터셋
uspto-grants-1998_12
특허 번호
US05849735

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