تفاعل #95337

معادلة التفاعل

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

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

sodium borohydride

sodium borohydride

→

desired product

المردود 82.6%

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

المردود 82.6%

المذيبات

methanol

ظروف التفاعل

المعالجة

1. 1
   workup.STIRRINGThen, the mixture is stirred overnight at room temperature
2. 2
   workup.STIRRINGstirred at room temperature for 3 hours
3. 3
   أخرىThe white crystals deposited are separated by filtration
4. 4
   غسيلwashed with methanol and water
5. 5
   أخرىdried
6. 6
   أخرىto obtain 2.36 g of a crude product
7. 7
   تركيزIn the meantime, the filtrate is concentrated under reduced pressure
8. 8
   workup.ADDITIONThe residue is mixed with water
9. 9
   أخرىThe crystals deposited are separated by filtration
10. 10
    غسيلwashed with water
11. 11
    أخرىdried
12. 12
    أخرىto obtain 0.37 g of a crude product
13. 13
    أخرىrecrystallized from ethanol

الإجراء التجريبي

In this example, 3.0 g of 1-(3,4-methylenedioxybenzoylmethyl)-4-(2-oxo-3,4-dihydro-2H-1,3-benzoxazin-3-yl)-piperidine obtained in Example 2 is mixed with 150 ml of methanol. While the mixture is stirred at 0° to 10° C., 0.8 g of sodium borohydride is added thereto over a period of 3 hours. Then, the mixture is stirred overnight at room temperature. The mixture is further mixed with 0.4 g of sodium borohydride and stirred at room temperature for 3 hours. The white crystals deposited are separated by filtration, washed with methanol and water and dried to obtain 2.36 g of a crude product. In the meantime, the filtrate is concentrated under reduced pressure. The residue is mixed with water. The crystals deposited are separated by filtration, washed with water and dried to obtain 0.37 g of a crude product. The two crude products are combined and recrystallized from ethanol to obtain 2.49 g of the desired product.

المصدر