반응 #95339

반응 방정식

1-(3,4,5-trimethoxybenzoylmethyl)-4-(2-oxo-3,4-dihydro-2H-1,3-benzoxazin-3-yl)-piperidine

sodium borohydride

sodium borohydride

→

desired product

수율 62.6%

1-[2-(3,4,5-Trimethoxyphenyl)-2-hydroxyethyl]-4-(2-oxo-3,4-dihydro-2H-1,3-benzoxazin-3-yl)-piperidine

수율 62.6%

용매

methanol

반응 조건

후처리

1. 1
   workup.STIRRINGThen, the mixture is stirred overnight at room temperature
2. 2
   workup.STIRRINGstirred overnight
3. 3
   기타The white crystals deposited are separated by filtration
4. 4
   세척washed with methanol and water
5. 5
   기타dried
6. 6
   기타to obtain 1.96 g of a crude product
7. 7
   기타The crude product is recrystallized from ethanol

실험 절차

In this example, 2.8 g of 1-(3,4,5-trimethoxybenzoylmethyl)-4-(2-oxo-3,4-dihydro-2H-1,3-benzoxazin-3-yl)-piperidine obtained in the same manner as in Example 7 is mixed with 150 ml of methanol. While this mixture is stirred at 0° to 10° C., 1.5 g of sodium borohydride is added thereto over a period of 2 hours. Then, the mixture is stirred overnight at room temperature. The mixture is further mixed with 1 g of sodium borohydride and stirred overnight. The white crystals deposited are separated by filtration, washed with methanol and water and dried to obtain 1.96 g of a crude product. The crude product is recrystallized from ethanol to obtain 1.76 g of the desired product.

출처