反应 #640575

ord-279427bedc5d4d239b00cc6dfc2c8131

反应方程式

O=C1OC(c2ccccc2)CCN1Cc1ccccc1[N+](=O)[O-]
3-(2-Nitrobenzyl)-6-phenyl-[1,3]-oxazinan-2-one
[Cl-].[NH4+]
ammonium chloride
O
water
Nc1ccccc1CN1CCC(c2ccccc2)OC1=O
3-(2-aminobenzyl)-6-phenyl-[1,3]-oxazinan-2-one
收率 99.3%

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度to reflux for 1.5 hours
  2. 2
    过滤the reaction mixture was filtered with suction
  3. 3
    萃取extracted with ethyl acetate
  4. 4
    洗涤The organic layer was washed with a saturated brine
  5. 5
    干燥dried over anhydrous sodium sulfate

实验过程

3-(2-Nitrobenzyl)-6-phenyl-[1,3]-oxazinan-2-one (1.59 g, 5.10 mmol), iron powder (1.42 g, 25.4 mmol), ammonium chloride (0.14 g, 2.62 mmol) were suspended in ethanol (30 ml) and water (15 ml) and heated to reflux for 1.5 hours. After cooling to room temperature, the reaction mixture was filtered with suction and extracted with ethyl acetate. The organic layer was washed with a saturated brine and then dried over anhydrous sodium sulfate, and 3-(2-aminobenzyl)-6-phenyl-[1,3]-oxazinan-2-one (1.43 g) was obtained by evaporating the solvent under reduced pressure.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08048825B2uspto-grants-2011_11