反応 #66039

反応方程式

methanesulfonyl chloride

behenyl alcohol

triethylamine

→

white crystal

1-docosanyl methanesulfonate

溶媒

tetrahydrofuran

反応条件

後処理

1. 1
   workup.STIRRINGfurther stirred for 30 minutes
2. 2
   workup.ADDITIONthe resulting mixture was ultrasonically dispersed for 15 minutes
3. 3
   workup.STIRRINGfurther stirred at room temperature for 4 hours
4. 4
   ろ過The dispersion was filtered under reduced pressure
5. 5
   洗浄a crystal was washed with 2 L of water
6. 6
   workup.STIRRINGThe resulting white crystal was stirred in 1.5 L of acetonitrile for one hour
7. 7
   ろ過filtered under reduced pressure
8. 8
   洗浄washed with 0.5 L of acetonitrile
9. 9
   その他The resulting crystal was dried under reduced pressure

実験手順

247.4 g of behenyl alcohol (1-docosanol) was dissolved in 640 mL of tetrahydrofuran, 116.1 mL of methanesulfonyl chloride was gradually added, and 64.7 mL of triethylamine was then added dropwise under ice cooling over 30 minutes. After stirring for one hour, the mixture was heated at 40° C. and further stirred for 30 minutes. The reaction mixture was poured into 3.5 L of ice water, and the resulting mixture was ultrasonically dispersed for 15 minutes and further stirred at room temperature for 4 hours. The dispersion was filtered under reduced pressure, and a crystal was washed with 2 L of water. The resulting white crystal was stirred in 1.5 L of acetonitrile for one hour, filtered under reduced pressure and then washed with 0.5 L of acetonitrile. The resulting crystal was dried under reduced pressure to obtain 303.4 g of a white crystal.

出典