Urea → HCID 23362017, compound

HRID 1082049Notes

Reaction equation

HRID 1082049 reaction equation
[CH3:1][CH:2]1[NH:7][C:6]2=[C:8]([NH2:12])[CH:9]=[CH:10][CH:11]=[C:5]2[O:4][CH2:3]1.N[C:14](N)=[O:15]>CCOCC.CCCCCC>[CH3:1][CH:2]1[N:7]2[C:14](=[O:15])[NH:12][C:8]3=[CH:9][CH:10]=[CH:11][C:5](=[C:6]23)[O:4][CH2:3]1

Participants

4

Reactant 2

HCID 1176UreaHCID 23362026HCID 23362026, compound

Product 1

HCID 23362017HCID 23362017, compoundYield 52.6%

Reagents, catalysts & solvents 1

HCID 21584099Diethylether hexaneSolvent

Procedure

3.3 g (0.02 mol) of 3-methyl-3,4-dihydro-1H-1,4-benzoxazin-5-amine are heated at 160°-165° C. in an oil bath for 1.5 hours in the presence of 1.7 g (0.028 mol) of urea. A solid is obtained which is taken up in a water/ether (50/50) mixture. The phases are separated, the organic phase is recovered, is washed, is dried and the solvent evaporated to dryness. The residue obtained is purified by chromatography on a column of silica gel, the eluent being ethyl ether. 2 g of product are obtained.

Workup

  1. customA solid is obtained which
  2. customThe phases are separated
  3. customthe organic phase is recovered
  4. washis washed
  5. customis dried
  6. customthe solvent evaporated to dryness
  7. customThe residue obtained
  8. customis purified by chromatography on a column of silica gel

Sources & evidence

ORD record
ord-19496c1f264d4a43bc81ada1cd6e0b95
Source dataset
uspto-grants-1996_12
Patent number
US05589476

Reaction notes

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