反応 #2664

反応方程式

product

3-formyl-6-hydroxy-5-methoxy benzonitrile

boron tribromide

→

expected product

収率 72.4%

3-formyl-5,6-dihydroxy benzonitrile

収率 72.4%

溶媒

dichloromethane

dichloromethane

反応条件

後処理

1. 1
   workup.WAITthe mixture stood for one night at ambient temperature
2. 2
   濃縮It was concentrated
3. 3
   温度cooled again to 0° C.
4. 4
   workup.ADDITION250 ml of a normal solution of hydrochloric acid were added
5. 5
   その他The crystallized product was separated out
6. 6
   洗浄washed with water
7. 7
   その他dried
8. 8
   その他then crystallized from an isopropanol

実験手順

18 g of the product of Step A and 400 ml of dichloromethane were mixed together under nitrogen and the mixture was cooled to 0° C. 150 ml of a molar solution of boron tribromide in dichloromethane were added and the mixture stood for one night at ambient temperature. It was concentrated, cooled again to 0° C. and 250 ml of a normal solution of hydrochloric acid were added. The crystallized product was separated out, washed with water, dried then crystallized from an isopropanol--water mixture (1-2) to obtain 12 g of the expected product.

出典