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

HRID 351849

반응식

HRID 351849 반응식
[CH3:1][O:2][C:3]1[CH:24]=[C:23]([O:25][CH3:26])[CH:22]=[CH:21][C:4]=1[CH2:5][N:6]1[C:12](=[O:13])[C:11]2[CH:14]=[C:15]([S:18][CH3:19])[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:39])=O>C1(C)C=CC=CC=1>[Cl:39][C:8]1[CH2:7][N:6]([CH2:5][C:4]2[CH:21]=[CH:22][C:23]([O:25][CH3:26])=[CH:24][C:3]=2[O:2][CH3:1])[C:12](=[O:13])[C:11]2[CH:14]=[C:15]([S:18][CH3:19])[CH:16]=[CH:17][C:10]=2[N:9]=1

참가 물질

5

반응물 3

HCID 7471Dimethyl-p-toluidineHCID 24813Phosphorus oxychlorideHCID 227134824-(2,4-Dimethoxy-benzyl)-7-methylsulfanyl-3,4-dihydro-1H-benzo[e][1,4]diazepine-2,5-dione

생성물 1

HCID 227134842-Chloro-4-(2,4-dimethoxy-benzyl)-7-methylsulfanyl-3,4-dihydro-benzo[e][1,4]diazepin-5-one

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
100 °C

실험 절차

4-(2,4-Dimethoxy-benzyl)-7-methylsulfanyl-3,4-dihydro-1H-benzo[e][1,4]diazepine-2,5-dione (630 mg, 1.7 mmol) and N,N-dimethyl-p-toluidine (489 μL, 3.4 mmol) were mixed in toluene (5 mL) and heated to 100° C. Then phosphorus oxychloride (170 μL, 1.9 mmol) was added dropwise and heating at 100° C. was continued for 1 h. The resulting dark red solution was used directly in the subsequent step.

후처리

  1. temperatureheating at 100° C.

출처 및 근거

ORD 기록
ord-be20683897304400a6363b07e996b88e
출처 데이터셋
uspto-grants-2004_06
특허 번호
US06743789B2

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