Methanol → HCID 21156212、化合物

反応式

[C:1]([N:5]1[C:19]2[C:20]3[C:7]([CH2:8][C@@H:9]4[C:14]([C:15]=3[CH:16]=[CH:17][CH:18]=2)=[CH:13][C@@H:12]([CH2:21][OH:22])[CH2:11][N:10]4[CH3:23])=[CH:6]1)([CH3:4])([CH3:3])[CH3:2].S(=O)(=O)(O)O.[OH-:29].[NH4+].[CH3:31]O>O>[C:1]([N:5]1[C:19]2[C:20]3[C:7]([CH2:8][C@@H:9]4[C@@:14]([O:29][CH3:31])([C:15]=3[CH:16]=[CH:17][CH:18]=2)[CH2:13][C@@H:12]([CH2:21][OH:22])[CH2:11][N:10]4[CH3:23])=[CH:6]1)([CH3:4])([CH3:3])[CH3:2]

参加物

実験手順

A solution of 6 g of 1-(t-butyl)-9,10-didehydro-6-methyl-8β-hydroxymethyl-ergoline, prepared as described in Example 1, in 500 ml of methanol and 5 ml of sulphuric acid was irradiated at 20° C. in a Pyrex flask with a Hanau PL 321 lamp for about 6 hours, until the absorption at 315 nm completely disappeared. The solution was diluted with iced water, made basic with ammonium hydroxide, evaporated to 100 ml and extracted with ethyl acetate. After evaporation of the solvent the residue was chromatographed in silica gel and on elution with 97:3 dichloromethane:methanol, 5 g of the title compound was isolated, m.p. 172 to 174° C. from acetone.