Phosgene → HCID 21533324, compound

HRID 1657401Notes

Reaction equation

HRID 1657401 reaction equation
[C:1]([Cl:4])(Cl)=[O:2].[CH2:5]1[C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=2[CH2:9][CH2:8][NH:7][O:6]1>C1(C)C=CC=CC=1>[CH2:5]1[C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=2[CH2:9][CH2:8][N:7]([C:1]([Cl:4])=[O:2])[O:6]1

Participants

4

Reactant 2

HCID 6371PhosgeneHCID 21533329HCID 21533329, compound

Product 1

HCID 21533324HCID 21533324, compoundYield 81.5%

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent

Procedure

To a solution of 15.9 g. of phosgene in anhydrous toluene a solution of 19.8 g. (0.135 mole) of 1,3,4,5-tetrahydro-2,3-benzoxazepine in the same solvent was added at 0° - 15°C with stirring. After 6 hours it was washed with H2O, dried over Na2SO4 and the solvent evaporated. Recrystallization from EtOH yielded 22.85 g. (81.5%) of the title compound.

Workup

  1. washAfter 6 hours it was washed with H2O
  2. dry with materialdried over Na2SO4
  3. customthe solvent evaporated
  4. customRecrystallization from EtOH
  5. customyielded 22.85 g

Sources & evidence

ORD record
ord-7026505e239f4cb2ad8de227af429da6
Source dataset
uspto-grants-1976_06
Patent number
US03960858

Reaction notes

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