HCID 23460477, compound → HCID 13341925, compound

HRID 2286854Notes

Reaction equation

HRID 2286854 reaction equation
[O:1]=[C:2]1[C:7]2[CH:8]=[C:9]([C:12](Cl)=[O:13])[CH:10]=[CH:11][C:6]=2[O:5][CH:4]([C:15]([Cl:18])([Cl:17])[Cl:16])[NH:3]1>C(O)CCC>[O:1]=[C:2]1[C:7]2[CH:8]=[C:9]([C:12]([O:1][CH2:2][CH2:7][CH2:6][CH3:11])=[O:13])[CH:10]=[CH:11][C:6]=2[O:5][CH:4]([C:15]([Cl:18])([Cl:17])[Cl:16])[NH:3]1

Participants

3

Reactant 1

HCID 23460477HCID 23460477, compound

Product 1

HCID 13341925HCID 13341925, compound

Reagents, catalysts & solvents 1

HCID 2631-ButanolSolvent

Procedure

A suspension of powdered 3,4-dihydro-4-oxo-2-trichloromethyl-2H-benzo[e]-[1,3]-oxazine-6-carbonyl chloride (5.0 g.) in n-butanol (100 ml.) was heated on a steam bath for 30 minutes. The solution was cooled to ambient temperature, and the solvent was evaporated under reduced pressure. The sticky solid residue was triturated with petroleum ether (b.p. 60°-80° C.), filtered, washed with petroleum ether and crystallised from n-butanol to give butyl 3,4-dihydro-4-oxo-2-trichloromethyl-2H-benzo[e]-[1,3]-oxazine-6-carboxylate, m.p. 134°-136° C.

Workup

  1. temperaturewas heated on a steam bath for 30 minutes
  2. customthe solvent was evaporated under reduced pressure
  3. customThe sticky solid residue was triturated with petroleum ether (b.p. 60°-80° C.)
  4. filtrationfiltered
  5. washwashed with petroleum ether
  6. customcrystallised from n-butanol

Sources & evidence

ORD record
ord-d08a9ae4242b4b8bbf295d59e6c3408c
Source dataset
uspto-grants-1981_05
Patent number
US04268510

Reaction notes

Loading…