Ammonium Hydroxide → Acenaphthene-1,2-dicarboximide

HRID 1973447

반응식

HRID 1973447 반응식
[CH:1]1([C:16]([OH:18])=O)[C:11]2=[C:12]3[C:7](=[CH:8][CH:9]=[CH:10]2)[CH:6]=[CH:5][CH:4]=[C:3]3[CH:2]1[C:13](O)=[O:14].[OH-].[NH4+:20]>>[CH:1]12[C:16](=[O:18])[NH:20][C:13](=[O:14])[CH:2]1[C:3]1[C:12]3[C:7](=[CH:8][CH:9]=[CH:10][C:11]2=3)[CH:6]=[CH:5][CH:4]=1

참가 물질

3

반응물 2

HCID 14923Ammonium HydroxideHCID 27543701,2-Acenaphthylenedicarboxylic acid, 1,2-dihydro-

생성물 1

HCID 21491653Acenaphthene-1,2-dicarboximide

반응 조건

온도
200 °C

실험 절차

5.5 Parts of acenaphthene-1,2-dicarboxylic acid is heated in an oil bath with an excess of concentrated ammonium hydroxide. After most of the excess of ammonium hydroxide has distilled off, the temperature of the oil bath is raised to 200° C. and it is maintained at that temperature for 45 minutes. The residual material is sublimed under vacuum (0.05-0.1 mm.) using an oil bath at 280° C. The resultant solid is recrystallized from ethanol to give acenaphthene-1,2-dicarboximide melting at about 242°-246° C.

후처리

  1. distillationAfter most of the excess of ammonium hydroxide has distilled off
  2. temperatureit is maintained at that temperature for 45 minutes
  3. customat 280° C
  4. customThe resultant solid is recrystallized from ethanol

출처 및 근거

ORD 기록
ord-1b7a22926b3049d7860d79389db5a896
출처 데이터셋
uspto-grants-1976_12
특허 번호
US03997572

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