Phosphorus oxychloride → 1,2-Dihydroindolo[1,7-ab][1,5]benzodiazepine hydrochloride

HRID 2052700노트

반응식

HRID 2052700 반응식
[CH:1]([NH:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[N:10]1[C:18]2[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=2)[CH2:12][CH2:11]1)=O.P(Cl)(Cl)([Cl:21])=O>>[ClH:21].[CH2:11]1[N:10]2[C:5]3[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=3[N:3]=[CH:1][C:17]3=[C:18]2[C:13](=[CH:14][CH:15]=[CH:16]3)[CH2:12]1

참가 물질

3

반응물 2

HCID 24813Phosphorus oxychlorideHCID 12519124N-[2-(2,3-Dihydro-1H-indol-1-yl)phenyl]formamide

생성물 1

HCID 125191341,2-Dihydroindolo[1,7-ab][1,5]benzodiazepine hydrochloride

실험 절차

A mixture of 14.0 g of 1-(2-formamidophenyl)indoline and 50 ml of fresh phosphorus oxychloride are stirred and heated under N2. The mixture is refluxed 4.0 hours, then left at room temperature 18 hours. Excess POCl3 is then removed, leaving a solid which is triturated and boiled with absolute ethanol. The mixture is stirred 1 hour to homogenize the fine solid, then filtered, washed with ethanol, and dried to afford 1,2-dihydroindolo[1,7-ab][1,5]benzodiazepine hydrochloride, m.p. 228°-230° C. dec.

후처리

  1. temperatureheated under N2
  2. temperatureThe mixture is refluxed 4.0 hours
  3. customExcess POCl3 is then removed
  4. customleaving a solid which
  5. customis triturated
  6. stirringThe mixture is stirred 1 hour
  7. stirringto homogenize the fine solid
  8. filtrationfiltered
  9. washwashed with ethanol
  10. customdried

출처 및 근거

ORD 기록
ord-046567728a214618b26597b57d28de06
출처 데이터셋
uspto-grants-1980_01
특허 번호
US04186199

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