反応 #95352

反応方程式

1-(3,4-methylenedioxybenzoylmethyl)-4-[3,4-dihydro-2(1H)-quinazolinon-1-yl]-piperidine

sodium borohydride

→

desired product

収率 64.1%

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

収率 64.1%

溶媒

methanol

反応条件

後処理

1. 1
   温度cooling
2. 2
   その他is brought back to room temperature
3. 3
   workup.STIRRINGstirred for 3 hours at room temperature
4. 4
   濃縮the reaction solution is concentrated
5. 5
   workup.ADDITIONThe resultant residue is mixed with 50 ml of water
6. 6
   抽出the mixture is extracted with ethyl acetate (100 ml×2 and 50 ml×1)
7. 7
   洗浄The extract is washed with water
8. 8
   その他dried
9. 9
   濃縮concentrated
10. 10
    workup.ADDITIONThe resultant viscous residue is mixed with 5 ml of methanol
11. 11
    その他The crystals deposited are separated by filtration
12. 12
    洗浄washed with methanol
13. 13
    その他dried
14. 14
    その他to obtain 2.05 g of a crude product
15. 15
    その他The crude product is recrystallized from hot ethanol

実験手順

In this example, 2.70 g of 1-(3,4-methylenedioxybenzoylmethyl)-4-[3,4-dihydro-2(1H)-quinazolinon-1-yl]-piperidine and 150 ml of methanol are mixed and stirred under ice-cooling. Then, 2.0 g of sodium borohydride is added to the stirred mixture over a period of one hour. Subsequently, the mixture is brought back to room temperature and stirred for 3 hours at room temperature and the reaction solution is concentrated. The resultant residue is mixed with 50 ml of water and the mixture is extracted with ethyl acetate (100 ml×2 and 50 ml×1). The extract is washed with water, dried and concentrated. The resultant viscous residue is mixed with 5 ml of methanol. The crystals deposited are separated by filtration, washed with methanol and dried to obtain 2.05 g of a crude product. The crude product is recrystallized from hot ethanol to obtain 1.74 g of the desired product.

出典