Triethylamine → HCID 68128176, Verbindung

Reaktionsgleichung

[CH2:1]1[C:11]2[N:10]3[C:12]4[CH:21]=[CH:20][N:19]=[CH:18][C:13]=4[C:14]4[CH2:15][CH2:16][CH:17]=[C:8]([C:9]=43)[CH:7]=[CH:6][C:5]=2[CH2:4][CH2:3][CH2:2]1.C(N(CC)CC)C.C(Cl)(=[O:33])C(C)C>ClCCl>[CH:8]([C:9]([CH:14]([CH3:15])[CH3:13])=[O:33])([CH3:17])[CH3:7].[CH2:1]1[C:11]2[N:10]3[C:12]4[CH:21]=[CH:20][N:19]=[CH:18][C:13]=4[C:14]4[CH2:15][CH2:16][CH:17]=[C:8]([C:9]=43)[CH:7]=[CH:6][C:5]=2[CH2:4][CH2:3][CH2:2]1

Komponenten

Versuchsvorschrift

To a solution of 5.5 g. of the product of Example 1 in 150 ml. of dichloromethane containing 25 ml. of triethylamine a solution of 4.2 ml. of isobutyryl chloride in approximately 25 ml. of dichloromethane is added dropwise, with constant stirring. On heating to reflux, the white precipitate originally formed redissolves. Refluxing is continued for 2 hours; the solution is cooled, washed with water and with saturated sodium bicarbonate, dried over anhydrous potassium carbonate, and stripped down to a dark gum, which is taken up in hexane, boiled and decolorized. After concentrating the clear solution tp 100 ml. and cooling, a gum separates which solidifies completely on standing. After 1 week, 1,2,3,4,8,9-hexahydropyrido[4', 3':2,3]indolo[1,7-ab][1]benzazepin isopropyl ketone, m.p. 122°-124°, is isolated.