반응 #640578

ord-b0ea6a79bffb414bbdee97d0b8a8168e

반응 방정식

CC1CCN(Cc2ccccc2[N+](=O)[O-])C(=O)OC1
6-Methyl-3-(2-nitrobenzyl)-[1,3]-oxazepan-2-one
[Cl-].[NH4+]
ammonium chloride
O
water
CC1CCN(Cc2ccccc2N)C(=O)OC1
3-(2-aminobenzyl)-6-methyl-[1,3]-oxazepan-2-one
수율 60.2%

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도to reflux for one hour
  2. 2
    여과the reaction mixture was filtered with suction
  3. 3
    추출extracted with ethyl acetate
  4. 4
    세척The organic layer was washed with a saturated brine
  5. 5
    건조dried over anhydrous sodium sulfate

실험 절차

6-Methyl-3-(2-nitrobenzyl)-[1,3]-oxazepan-2-one (1.91 g, 7.23 mmol), iron powder (2.02 g, 36.2 mmol), ammonium chloride (0.19 g, 3.55 mmol) were suspended in ethanol (30 ml) and water (15 ml) and heated to reflux for one hour. 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-methyl-[1,3]-oxazepan-2-one (1.02 g) was obtained by evaporating the solvent under reduced pressure.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08048825B2uspto-grants-2011_11