Triethylamine → N-[4-[(5,11-dihydro-10H-dibenz[b,e](1,4]diazepin-5-yl)carbonyl]phenyl]-2-methylbenzamide

HRID 962597노트

반응식

HRID 962597 반응식
[CH:1]1[C:11]2[CH2:10][NH:9][C:8]3[CH:12]=[CH:13][CH:14]=[CH:15][C:7]=3[NH:6][C:5]=2[CH:4]=[CH:3][CH:2]=1.[CH3:16][C:17]1[CH:34]=[CH:33][CH:32]=[CH:31][C:18]=1[C:19]([NH:21][C:22]1[CH:30]=[CH:29][C:25]([C:26](Cl)=[O:27])=[CH:24][CH:23]=1)=[O:20].C(N(CC)CC)C>CN(C)C1C=CN=CC=1.C(Cl)Cl>[CH:1]1[C:11]2[CH2:10][NH:9][C:8]3[CH:12]=[CH:13][CH:14]=[CH:15][C:7]=3[N:6]([C:26]([C:25]3[CH:24]=[CH:23][C:22]([NH:21][C:19](=[O:20])[C:18]4[CH:31]=[CH:32][CH:33]=[CH:34][C:17]=4[CH3:16])=[CH:30][CH:29]=3)=[O:27])[C:5]=2[CH:4]=[CH:3][CH:2]=1

참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 3604610,11-Dihydro-5h-dibenzo[b,e][1,4]diazepineHCID 107074414-[(2-methylbenzoyl)amino]benzoyl Chloride

생성물 1

HCID 67624893N-[4-[(5,11-dihydro-10H-dibenz[b,e](1,4]diazepin-5-yl)carbonyl]phenyl]-2-methylbenzamide

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 6344Dichloromethane용매

실험 절차

A mixture of 1.0 g of 5,11-dihydro-10H-dibenz [b,e] [1,4]diazepine 1.9 g of 4-[(2-methylbenzoyl) amino]benzoyl chloride, 4 ml of triethylamine and 0.2 g of 4-(dimethylamino)pyridine in 60 ml of methylene chloride is stirred at room temperature for 18 hours. The reaction mixture is poured into ice water and the separated organic layer washed with 50 ml each of water, 2N HCl, water, saturated NaHCO3 and water. The organic layer is dried (Na2SO4) and the solvent removed to give a residue. The residue is chromatographed on a silica gel column using 1:4 ethyl acetate-hexane to give 1.8 g of the desired product as a solid, m.p. 68°-71° C.

후처리

  1. washthe separated organic layer washed with 50 ml each of water, 2N HCl, water, saturated NaHCO3 and water
  2. dry with materialThe organic layer is dried (Na2SO4)
  3. customthe solvent removed
  4. customto give a residue
  5. customThe residue is chromatographed on a silica gel column

출처 및 근거

ORD 기록
ord-18fe0cefdc9e437f9590799a74919879
출처 데이터셋
uspto-grants-1998_06
특허 번호
US05760031

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