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

HRID 981050ノート

反応式

HRID 981050 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 20071536HCID 20071536、化合物

試薬・触媒・溶媒 1

HCID 80192-Methoxyethanol溶媒

反応条件

温度
100 °C

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-1b2ad66461f24e86b081e58d7959bd32
出典データセット
uspto-grants-1991_02
特許番号
US04990510

反応ノート

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