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

HRID 2052700ノート

反応式

HRID 2052700 の反応式
[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

参加物

3

反応物 2

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

生成物 1

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

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-046567728a214618b26597b57d28de06
出典データセット
uspto-grants-1980_01
特許番号
US04186199

反応ノート

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