Methyl Bromide → Tri-o-thymotide methyl bromide
反応式
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([CH3:10])[CH3:9])=[C:4]2[O:11][C:12]([C:14]3[C:19]([O:20][C:21]([C:23]4[C:28]([O:29][C:30](=[O:31])[C:3]=12)=[C:27]([CH:32]([CH3:34])[CH3:33])[CH:26]=[CH:25][C:24]=4[CH3:35])=[O:22])=[C:18]([CH:36]([CH3:38])[CH3:37])[CH:17]=[CH:16][C:15]=3[CH3:39])=[O:13].[CH3:40][Br:41]>CC(C)(CC(C)C)C>[CH3:39][C:15]1[CH:16]=[CH:17][C:18]([CH:36]([CH3:38])[CH3:37])=[C:19]2[O:20][C:21]([C:23]3[C:28]([O:29][C:30]([C:3]4[C:4]([O:11][C:12](=[O:13])[C:14]=12)=[C:5]([CH:8]([CH3:9])[CH3:10])[CH:6]=[CH:7][C:2]=4[CH3:1])=[O:31])=[C:27]([CH:32]([CH3:34])[CH3:33])[CH:26]=[CH:25][C:24]=3[CH3:35])=[O:22].[CH3:40][Br:41]参加物
4
実験手順
Tri-o-thymotide (25 g) was dissolved in 2,2,4-trimethylpentane (50 ml) at 100° C. and the hot solution was introduced into the high pressure autoclave. Methyl bromide was added to the autoclave until a pressure of 200 bar was reached. The high pressure autoclave was then kept for 2 hours at 110° C. and the solution was then cooled down to room temperature within 5 days. The crystals were filtered off and washed 3 times with cold 2,2,4-trimethylpentane. The crystals were then dried in the drying cabinet at 50° C.