8-nitro-3,4-dihydro-2H-1,5-benzodioxepin-7-amine → 81864-63-3

HRID 1903172Notes

Reaction equation

HRID 1903172 reaction equation
[NH2:1][C:2]1[C:12]([N+:13]([O-])=O)=[CH:11][C:5]2[O:6][CH2:7][CH2:8][CH2:9][O:10][C:4]=2[CH:3]=1>CO.[Ni]>[O:6]1[C:5]2[CH:11]=[C:12]([NH2:13])[C:2]([NH2:1])=[CH:3][C:4]=2[O:10][CH2:9][CH2:8][CH2:7]1

Participants

4

Reactant 1

HCID 42520338-nitro-3,4-dihydro-2H-1,5-benzodioxepin-7-amine

Product 1

HCID 912071381864-63-3Yield 88.1%

Reagents, catalysts & solvents 2

HCID 935NickelCatalystHCID 887MethanolSolvent

Procedure

10.2 g of 7-amino-8-nitro-3,4-dihydro-2H-1,5-benzodioxepine were hydrogenated in 500 ml of methanol with Raney-nickel. After separating the catalyst, the solution was evaporated and the residue was recrystallized from ethyl acetate/petroleum either (low boiling). 7.7 g of 3,4-dihydro-2H-1,5-benzodioxepine-7,8-diamine (88.0% of theory) of melting point 97°-102° C. were obtained.

Workup

  1. customAfter separating the catalyst
  2. customthe solution was evaporated
  3. customthe residue was recrystallized from ethyl acetate/petroleum either (low boiling)

Sources & evidence

ORD record
ord-b37dd8e3ca7d44a09f6e50e3c2be8ac6
Source dataset
uspto-grants-1984_03
Patent number
US04435406

Reaction notes

Loading…