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N,N-Dimethylaniline → 5-Chloro-7,8-dimethoxy-1-methyl-1,3-dihydro-1,4-benzodiazepin-2-one

HRID 1297096
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HRID 1297096 반응식
[CH3:1][O:2][C:3]1[C:4]([O:17][CH3:18])=[CH:5][C:6]2[N:12]([CH3:13])[C:11](=[O:14])[CH2:10][NH:9][C:8](=O)[C:7]=2[CH:16]=1.CN(C)C1C=CC=CC=1.O=P(Cl)(Cl)[Cl:30].C(Cl)Cl>C(Cl)(Cl)Cl.C(N(CC)CC)C>[Cl:30][C:8]1[C:7]2[CH:16]=[C:3]([O:2][CH3:1])[C:4]([O:17][CH3:18])=[CH:5][C:6]=2[N:12]([CH3:13])[C:11](=[O:14])[CH2:10][N:9]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 949N,N-DimethylanilineHCID 6344DichloromethaneHCID 24813Phosphorus oxychlorideHCID 691555977,8-dimethoxy-1-methyl-3,4-dihydro-1H-1,4-benzodiazepine-2,5-dione

생성물 1

HCID 691548525-Chloro-7,8-dimethoxy-1-methyl-1,3-dihydro-1,4-benzodiazepin-2-one

시약·촉매·용매 2

HCID 6212
이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트
Chloroform
용매
HCID 8471Triethylamine용매

실험 절차

Heat at 125° C. in a sealed tube for 3Y4 hour a solution of 100 mg (0.40 mmol) of 7,8-dimethoxy-1-methyl-3,4-dihydro-1H-1,4-benzodiazepine-2,5-dione (XVIIaa), 280 μl of dimethylaniline, 800 μl of POCl3, in 10 ml of anhydrous CHCl3. Allow to cool to room temperature. Add 3 g of silica and 5 ml of CH2Cl2. Add at 0° C., 1 ml of triethylamine.

후처리

  1. additionAdd at 0° C.

출처 및 근거

ORD 기록
ord-70924f78099548cd8820a2a050bcdd2a
출처 데이터셋
uspto-grants-2007_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07250410B2

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