반응 #3863

반응 방정식

Piperidine

Methane sulfonyl chloride

product

6-Methoxy-4-hydroxy-2,3-dihydrobenzopyran

sodium bicarbonate

→

desired product

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

용매

methylene chloride

triethylamine

반응 조건

후처리

1. 1
   온도cooled to 0° C
2. 2
   workup.STIRRINGthe solution stirred at RT overnight
3. 3
   workup.STIRRINGthe mixture is stirred for 30 minutes
4. 4
   기타The organic layer is separated
5. 5
   세척washed with sat'd NaCl
6. 6
   기타dried
7. 7
   여과The solution is filtered
8. 8
   기타the filtrate evaporated in vacuo

실험 절차

Methane sulfonyl chloride (14.9 ml) is added dropwise to a stirred 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 at RT for 21/2 hours and cooled to 0° C. Piperidine (175 ml) is added to the cooled reaction mixture and the solution stirred at RT overnight. Sat'd aq. sodium bicarbonate is added to the solution and the mixture is stirred for 30 minutes. The organic layer is separated, washed with sat'd NaCl and dried. The solution is filtered and the filtrate evaporated in vacuo yielding the desired product as its hydrochloride salt.

출처