反応 #43971

反応方程式

sodium hydroxide

D-sorbitol

allyl chloride

allyl chloride

allyl chloride

→

Sorbitol Allyl Ether

反応条件

後処理

1. 1
   その他At 3.7 hours after the initiation of the reaction
2. 2
   workup.ADDITIONThen the addition
3. 3
   その他after the initiation of the reaction
4. 4
   その他is separated so that an oil layer
5. 5
   workup.ADDITIONfor adding total amount of 459 g of allyl chloride
6. 6
   workup.WAITwas 8 hours
7. 7
   その他after the initiation of the reaction
8. 8
   workup.WAITwas 11 hours
9. 9
   その他after the initiation of the reaction
10. 10
    その他was between 70° C. and 90° C
11. 11
    workup.WAITAfter the mixture was digested for one hour
12. 12
    温度the mixture was cooled

実験手順

At 3.7 hours after the initiation of the reaction, the addition of 200 g of allyl chloride was completed. Then the addition was continued. The time required for adding 300 g of allyl chloride was 5.5 hours after the initiation of the reaction. At this point of time (at the time at which allyl halide was added in the amount of 20% by mol, based on total molar number of hydroxyl group contained in D-sorbitol), the reflux liquid is separated so that an oil layer alone is returned to the reactor by attaching a water metering reservoir between the reflux condenser and the reactor. The time required for adding total amount of 459 g of allyl chloride was 8 hours after the initiation of the reaction. At this point of time, the dropwise addition of 333 g of 48% aqueous sodium hydroxide solution from the other dropping funnel was initiated. The time required for adding total amount of 842 g of allyl chloride was 11 hours after the initiation of the reaction. The temperature was between 70° C. and 90° C. After the mixture was digested for one hour, the mixture was cooled.

出典