反応 #3866

反応方程式

Methane sulfonyl chloride

product

4-Hydroxy-8-methoxy-2,3-dihydrobenzopyran

triethylamine

piperidine

→

desired product

8-Methoxy-4-piperidino-2,3-dihydrobenzopyran

溶媒

methylene chloride

反応条件

後処理

1. 1
   workup.STIRRINGthe reaction mixture is stirred under nitrogen overnight
2. 2
   洗浄The reaction mixture is washed with sat'd aq. sodium bicarbonate
3. 3
   その他dried
4. 4
   ろ過filtered
5. 5
   その他evaporated in vacuo

実験手順

Methane sulfonyl chloride (14.9 ml) is added dropwise to a solution of the product obtained in Step 1. (31.6 g) and triethylamine (29.3 ml) in methylene chloride (750 ml) cooled to 0° C. under nitrogen. The reaction mixture is stirred for 11/2 hours; piperidine (175 ml) is added and the reaction mixture is stirred under nitrogen overnight. The reaction mixture is washed with sat'd aq. sodium bicarbonate, sat'd NaCl, dried, filtered and evaporated in vacuo yielding the desired product as its hydrochloride salt.

出典