反応 #2756
ord-c8bd279ef8414749819522d3b3ae0914
反応条件
詳細条件
See reaction.notes.procedure_details.
後処理
- 1workup.ADDITIONthe hot solution was introduced into the high pressure autoclave
- 2ろ過The crystals were filtered off
- 3洗浄washed 3 times with cold 2,2,4-trimethylpentane
- 4その他The crystals were then dried in the drying cabinet at 50° C.
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.