反応 #458710

反応方程式

3-chloro-2,4,6-trimethyl-benzyl-triphenylphosphonium chloride

7-formyl-3-methyl-octa-2,4,6-trien-1-oic acid butyl ester

1,2-butylene oxide

→

3,7-dimethyl-nona-2,4,6,8-tetraen-1-oic acid butyl ester

反応条件

後処理

1. 1
   workup.DISTILLATIONThe 1,2-butylene oxide is slowly distilled off
2. 2
   workup.STIRRINGThe reaction mixture is stirred for 30 minutes at 80°-82° C.
3. 3
   温度cooled
4. 4
   抽出thoroughly extracted with hexane
5. 5
   抽出The hexane extract
6. 6
   workup.STIRRINGis shaken out 5 times with 50 ml of methanol/water 70:30 parts by volume each time
7. 7
   乾燥dried over sodium sulphate
8. 8
   その他evaporated under reduced pressure

実験手順

16 g of 3-chloro-2,4,6-trimethyl-benzyl-triphenylphosphonium chloride and 10 g of 7-formyl-3-methyl-octa-2,4,6-trien-1-oic acid butyl ester are heated to boiling with stirring after the addition of 40 g of 1,2-butylene oxide. The 1,2-butylene oxide is slowly distilled off. The reaction mixture is stirred for 30 minutes at 80°-82° C., then cooled and thoroughly extracted with hexane. The hexane extract is shaken out 5 times with 50 ml of methanol/water 70:30 parts by volume each time, then dried over sodium sulphate and evaporated under reduced pressure to produce 9-(3-chloro-2,4,6-trimethyl-phenyl), 3,7-dimethyl-nona-2,4,6,8-tetraen-1-oic acid butyl ester as a residue.

出典