Sodium Chloride → HCID 19036607、化合物

反応式

[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]2[C:14]3[N:13]([CH2:15][CH2:16][NH:17][C:18](=[O:20])[CH3:19])[CH:12]=[CH:11][C:10]=3[CH2:9][CH2:8][C:7]=2[CH:21]=1.[OH-:22].[K+].[Cl-].[Na+].[CH2:26]([OH:29])[CH2:27]O.[OH2:30]>>[C:18]([OH:20])(=[O:30])/[CH:19]=[CH:27]/[C:26]([OH:29])=[O:22].[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]2[C:14]3[N:13]([CH2:15][CH2:16][NH2:17])[CH:12]=[CH:11][C:10]=3[CH2:9][CH2:8][C:7]=2[CH:21]=1

参加物

反応物 4

HCID 5234Sodium Chloride

HCID 14797Potassium Hydroxide

HCID 19036463HCID 19036463、化合物

HCID 20437942Ethylene glycol water

生成物 1

HCID 19036607HCID 19036607、化合物収率 38%

実験手順

0.5 g of N-[2-(4,5-dihydro-7-methoxy-1H-benz[g]indol-1-yl)ethyl]-acetamide were heated to 140° for 23 hours under argon in 21 ml of ethylene glycol/water 2:1 in the presence of 0.60 g of potassium hydroxide. The reaction mixture was left to cool and poured into 100 ml of semi-concentrated sodium chloride solution. The mixture was extracted three times with diethyl ether. The combined extracts were washed once with saturated sodium chloride solution, dried over sodium sulfate, filtered and evaporated. The crude product was dissolved in 20 ml of diethyl ether and added dropwise to a solution of 245 mg of fumaric acid in 20 ml of methanol. The mixture was left to stir for one hour. and the yellowish crystals were filtered off under suction. 241 mg (38%) of 2-(4,5-dihydro-7-methoxy-1H-benz[g]indol-1-yl)-ethylamine fumarate (1:0.8) with m.p. 195° were obtained.