反応 #43298

反応方程式

NaOH

intermediate ( 7 )

methyl 3,4-dihydro-9-methoxy-2H-1,5-benzodioxepin-6-carboxylate

→

9-methoxy-3,4-dihydro-2H-1,5-benzodioxepin-6-carboxylic acid

溶媒

THF

反応条件

後処理

1. 1
   その他The solvent was evaporated partially
2. 2
   その他The mixture was separated into its layers
3. 3
   ろ過The solid was filtered off
4. 4
   洗浄washed with water
5. 5
   その他dried

実験手順

A NaOH solution (500 ml, 2N) was added to a solution of intermediate (7) in THF (250 ml). The mixture was stirred at room temperature overnight. The solvent was evaporated partially. The residue was extrated with DCM. The mixture was separated into its layers. The aqueous layer was acidified with a concentrated HCl solution until pH=1 to 2. The solid was filtered off, washed with water and dried, yielding 35.5 g of 9-methoxy-3,4-dihydro-2H-1,5-benzodioxepin-6-carboxylic acid (intermediate 8).

出典