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Methanol → HCID 178419254, 화합물

HRID 1382534
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HRID 1382534 반응식
[CH2:1]([N:3]([CH2:38][CH3:39])[CH2:4][CH2:5][N:6]1[C:14]2[CH:13]=[CH:12][C:11]([NH:15][CH2:16][CH2:17][N:18]3[C:26](=[O:27])[C:25]4[C:20](=[CH:21][CH:22]=[CH:23][CH:24]=4)[C:19]3=[O:28])=[C:10]3[S:29][C:30]4[CH:35]=[C:34]([O:36]C)[CH:33]=[CH:32][C:31]=4[C:8]([C:9]=23)=[N:7]1)[CH3:2].B(Br)(Br)[Br:41].CO>ClCCl>[BrH:41].[BrH:41].[CH2:38]([N:3]([CH2:1][CH3:2])[CH2:4][CH2:5][N:6]1[C:14]2[CH:13]=[CH:12][C:11]([NH:15][CH2:16][CH2:17][N:18]3[C:19](=[O:28])[C:20]4[C:25](=[CH:24][CH:23]=[CH:22][CH:21]=4)[C:26]3=[O:27])=[C:10]3[S:29][C:30]4[CH:35]=[C:34]([OH:36])[CH:33]=[CH:32][C:31]=4[C:8]([C:9]=23)=[N:7]1)[CH3:39]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 887MethanolHCID 25134Boron tribromide2회HCID 144067742-[2-[[2-[2-(Diethylamino)ethyl]-8-methoxy-2H-[1]benzothiopyrano[4,3,2-cd]indazol-5-yl]amino]ethyl]-1H-isoindole-1,3(2H)-dione

생성물 1

HCID 178419254HCID 178419254, 화합물수율 70.8%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

A 25° C. solution of 324.1 g (0.598 mol) of 2-[2-[[2-[2-(diethylamino)ethyl]-8-methoxy-2H-[1]benzothiopyrano[4,3,2-cd]indazol-5-yl]amino]ethyl]-1H-isoindole-1,3(2H)-dione (2) in 7.45 L of dichloromethane was treated dropwise over 2 hr with 2.1 L (2.1 mol) of a 1M solution of boron tribromide in dichloromethane. The mixture was heated at reflux for 6.75 hr, treated with an additional 300 mL (0.3 mol) of boron tribromide solution, then further heated overnight. The refluxing mixture was treated cautiously with 1.86 L of methanol, heated an additional 12 hr, then cooled and stirred for 3 hr in an ice bath. The solids were collected by filtration, washed successively with dichloromethane and hexane, then dried at 220 mm/45° C./20 hr to give 291.8 g (70.8%) of 3, mp 232.5°- 234° C., 98.9% pure by HPLC.

후처리

  1. temperatureThe mixture was heated
  2. temperatureat reflux for 6.75 hr
  3. temperaturefurther heated overnight
  4. temperatureheated an additional 12 hr
  5. temperaturecooled
  6. filtrationThe solids were collected by filtration
  7. washwashed successively with dichloromethane and hexane
  8. customdried at 220 mm/45° C./20 hr

출처 및 근거

ORD 기록
ord-720248306ade409c97e9af510acf7812
출처 데이터셋
uspto-grants-1989_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04806654

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