Methanol → HCID 22142321、化合物

反応式

[Cl:1][C:2]1[CH:3]=[C:4]([CH3:18])[C:5]2[O:9][C:8]([N:10]3[CH2:16][CH2:15][CH2:14][NH:13][CH2:12][CH2:11]3)=[N:7][C:6]=2[CH:17]=1.[CH3:19][S:20]([OH:23])(=[O:22])=[O:21].CO.CO.CS(O)(=O)=O>C(OCC)(=O)C>[CH3:19][S:20]([OH:23])(=[O:22])=[O:21].[Cl:1][C:2]1[CH:3]=[C:4]([CH3:18])[C:5]2[O:9][C:8]([N:10]3[CH2:16][CH2:15][CH2:14][NH:13][CH2:12][CH2:11]3)=[N:7][C:6]=2[CH:17]=1

参加物

実験手順

A solution of 5-chloro-2-(1-homopiperazinyl)-7-methylbenzoxazole (2.5 g) in ethyl acetate (75 mL) was added dropwise with a separately prepared methanesulfonic acid/methanol solution [prepared by adding methanol to methanesulfonic acid (0.61 mL) to a total volume of 12.5 mL] at room temperature with stirring. After the addition, the mixture was stirred for 1 hour at room temperature and for 1 hour with ice cooling, and the produced colorless precipitates were collected by filtration. The precipitates were dried under reduced pressure at 4 C.° for 5 hours to obtain the title compound (3.0 g).