Dimethyl-p-toluidine → 2-Chloro-4-(2,4-dimethoxy-benzyl)-7-bromo-3,4-dihydro-benzo[e][1,4]diazepin-5-one

HRID 351841노트

반응식

HRID 351841 반응식
[CH3:1][O:2][C:3]1[CH:23]=[C:22]([O:24][CH3:25])[CH:21]=[CH:20][C:4]=1[CH2:5][N:6]1[C:12](=[O:13])[C:11]2[CH:14]=[C:15]([Br:18])[CH:16]=[CH:17][C:10]=2[NH:9][C:8](=O)[CH2:7]1.CN(C)C1C=CC(C)=CC=1.P(Cl)(Cl)([Cl:38])=O>C1(C)C=CC=CC=1>[Cl:38][C:8]1[CH2:7][N:6]([CH2:5][C:4]2[CH:20]=[CH:21][C:22]([O:24][CH3:25])=[CH:23][C:3]=2[O:2][CH3:1])[C:12](=[O:13])[C:11]2[CH:14]=[C:15]([Br:18])[CH:16]=[CH:17][C:10]=2[N:9]=1

참가 물질

5

반응물 3

HCID 7471Dimethyl-p-toluidineHCID 24813Phosphorus oxychlorideHCID 227134707-Bromo-4-(2,4-dimethoxybenzyl)-3,4-dihydro-1H-benzo[e][1,4]diazepine-2,5-dione

생성물 1

HCID 227134852-Chloro-4-(2,4-dimethoxy-benzyl)-7-bromo-3,4-dihydro-benzo[e][1,4]diazepin-5-one

시약·촉매·용매 1

HCID 1140Toluene용매

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온도
100 °C

실험 절차

4-(2,4-Dimethoxy-benzyl)-7-bromo-3,4-dihydro-1H-benzo[e][1,4]diazepine-2,5-dione (3.0 g, 7.4 mmol) and N,N-dimethyl-p-toluidine (2.1 mL, 14.8 mmol) were mixed in toluene (30 mL) and heated to 100° C. Then phosphorus oxychloride (745 μL, 8.1 mmol) was added dropwise and heating at 100° C. was continued for 2.5 h. The resulting dark red solution was evaporated and the residue dissolved in THF (10 mL) and used directly in the subsequent step.

후처리

  1. temperatureheating at 100° C.
  2. customThe resulting dark red solution was evaporated
  3. dissolutionthe residue dissolved in THF (10 mL)

출처 및 근거

ORD 기록
ord-6b8915960bd74c35be7caac5e7f40218
출처 데이터셋
uspto-grants-2004_06
특허 번호
US06743789B2

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