Hydrochloric Acid → 8-chloro-10,11-dihydro-10-[(1,3-dihydro-1,3-dioxo-2H-isoindol-2-yl)acetyl]dibenz[b,f][1,4]oxazepine

HRID 248821

반응식

HRID 248821 반응식
[CH:1]1[CH:6]=[C:5]2[C:7]([N:9]([CH2:12][C:13](Cl)=[O:14])[C:10](=[O:11])[C:4]2=[CH:3][CH:2]=1)=[O:8].[Cl:16][C:17]1[CH:31]=[CH:30][C:20]2[O:21][C:22]3[CH:29]=[CH:28][CH:27]=[CH:26][C:23]=3[CH2:24][NH:25][C:19]=2[CH:18]=1.C(N(CC)CC)C.Cl>C1(C)C=CC=CC=1>[Cl:16][C:17]1[CH:31]=[CH:30][C:20]2[O:21][C:22]3[CH:29]=[CH:28][CH:27]=[CH:26][C:23]=3[CH2:24][N:25]([C:13](=[O:14])[CH2:12][N:9]3[C:7](=[O:8])[C:5]4[C:4](=[CH:3][CH:2]=[CH:1][CH:6]=4)[C:10]3=[O:11])[C:19]=2[CH:18]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 812422H-Isoindole-2-acetyl chloride, 1,3-dihydro-1,3-dioxo-HCID 152292278-Chloro-10,11-dihydrodibenzo[b,f][1,4]oxazepine

생성물 1

HCID 106697298-chloro-10,11-dihydro-10-[(1,3-dihydro-1,3-dioxo-2H-isoindol-2-yl)acetyl]dibenz[b,f][1,4]oxazepine

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

1,3-dihydro-1,3-dioxo-2H-isoindole-2-acetyl chloride (4.00 grams), 8-chloro-10,11-dihydrodibenz[b,f][1,4]oxazepine (4.16 grams) and triethylamine (2.8 mL) were refluxed in toluene (100 mL) under nitrogen for 3 hours. The resulting mixture was poured into 1N HCl at 0° C., and the biphasic mixture was shaken vigorously. The insoluble product was collected by filtration, washed with toluene and ethyl ether, and dried in vacuo at 56° C. The yield of the title compound was 6.36 grams (85%). Mp: 184°-185° C.

후처리

  1. filtrationThe insoluble product was collected by filtration
  2. washwashed with toluene and ethyl ether
  3. customdried in vacuo at 56° C

출처 및 근거

ORD 기록
ord-9756dccc208d4fa6826e9969be32adff
출처 데이터셋
uspto-grants-1993_05
특허 번호
US05212169

연결된 노트

불러오는 중…