반응 #3866

반응 방정식

Methane sulfonyl chloride

product

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

triethylamine

piperidine

→

desired product

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

용매

methylene chloride

반응 조건

후처리

1. 1
   workup.STIRRINGthe reaction mixture is stirred under nitrogen overnight
2. 2
   세척The reaction mixture is washed with sat'd aq. sodium bicarbonate
3. 3
   기타dried
4. 4
   여과filtered
5. 5
   기타evaporated in vacuo

실험 절차

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.

출처