9-Chloro-6H-indolo[2,3-b]quinoxaline → HCID 20071536, 화합물

HRID 981050노트

반응식

HRID 981050 반응식
[Na].Cl.[CH3:3][N:4]([CH2:6][CH2:7][Cl:8])[CH3:5].[Cl:9][C:10]1[CH:15]=[CH:14][C:13]2[NH:16][C:17]3[C:26]([C:12]=2[CH:11]=1)=[N:25][C:24]1[C:19](=[CH:20][CH:21]=[CH:22][CH:23]=1)[N:18]=3>COCCO>[ClH:8].[Cl:9][C:10]1[CH:15]=[CH:14][C:13]2[N:16]([CH2:7][CH2:6][N:4]([CH3:3])[CH3:5])[C:17]3[C:26]([C:12]=2[CH:11]=1)=[N:25][C:24]1[C:19](=[CH:20][CH:21]=[CH:22][CH:23]=1)[N:18]=3

참가 물질

5

반응물 3

HCID 52938709-Chloro-6H-indolo[2,3-b]quinoxalineHCID 5360545SodiumHCID 11636816N,N-Dimethylaminoethyl chloride hydrochloride

생성물 1

HCID 20071536HCID 20071536, 화합물

시약·촉매·용매 1

HCID 80192-Methoxyethanol용매

반응 조건

온도
100 °C

실험 절차

5.06 g sodium (0.22 mole) is dissolved in 300 ml 2-methoxyethanol, 15.9 g N,N-dimethylamino-2-chloroethane-HCl (0.11 mole) is added followed by 25.4 g 9-chloro-6H-indolo(2,3-b)quinoxaline (0.10 mole). The mixture is heated for 3 hours at 100° C., cooled and filtered. The filtrate is concentrated and poured into water. The raw base obtained is filtered off and washed with water and subjected to chromatography on silica gel with methanol as eluent. The purified base is dissolved after drying in acetone. The hydrochloride is precipitated by slowly dropwise adding concentrated hydrochloric acid with stirring. Yield 23.2 g, 66%, mp. 243°-246° C.

후처리

  1. temperaturecooled
  2. filtrationfiltered
  3. concentrationThe filtrate is concentrated
  4. additionpoured into water

출처 및 근거

ORD 기록
ord-1b2ad66461f24e86b081e58d7959bd32
출처 데이터셋
uspto-grants-1991_02
특허 번호
US04990510

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