반응 #95338

반응 방정식

1-[1-(3,4-dimethoxybenzoyl)-ethyl]-4-(2-oxo-3,4-dihydro-2H-1,3-benzoxazin-3-yl)-piperidine

1-[1 -(3,4-Dimethoxybenzoyl)-ethyl]-4-(2-oxo-3,4-dihydro-2H-1,3-benzoxazin-3-yl)-piperidine

sodium borohydride

→

desired product

수율 59.4%

1-[3-(3,4-Dimethoxyphenyl)-3-hydroxypropan-2-yl]-4-(2-oxo-3,4-dihydro-2H-1,3-benzoxazin-3-yl)-piperidine

수율 59.4%

용매

methanol

반응 조건

후처리

1. 1
   workup.STIRRINGThe mixture is further stirred for 3 hours at the same temperature
2. 2
   workup.STIRRINGstirred overnight at room temperature
3. 3
   기타The white crystals deposited are separated by filtration
4. 4
   세척washed with methanol and water
5. 5
   기타dried
6. 6
   기타to obtain 1.90 g of a crude product
7. 7
   기타The crude product is recrystallized from ethanol

실험 절차

In this example, 2.8 g of 1-[1-(3,4-dimethoxybenzoyl)-ethyl]-4-(2-oxo-3,4-dihydro-2H-1,3-benzoxazin-3-yl)-piperidine obtained in Example 5 is mixed with 150 ml of methanol. While the mixture is stirred at 0° to 10° C., 2 g of sodium borohydride is added thereto over a period of one hour. The mixture is further stirred for 3 hours at the same temperature and then stirred overnight at room temperature. The white crystals deposited are separated by filtration, washed with methanol and water and dried to obtain 1.90 g of a crude product. The crude product is recrystallized from ethanol to obtain 1.67 g of the desired product.

출처