Potassium Carbonate → HCID 20203314, compound

HRID 1632949Notes

Reaction equation

HRID 1632949 reaction equation
Cl.[CH3:2][O:3][NH2:4].C(=O)([O-])[O-:6].[K+].[K+].[F:11][C:12]([F:23])([F:22])[C:13]1[CH:21]=[CH:20][CH:19]=[CH:18][C:14]=1[C:15](Cl)=[O:16]>>[CH3:2][O:3][N:4]([C:15](=[O:16])[C:14]1[CH:18]=[CH:19][CH:20]=[CH:21][C:13]=1[C:12]([F:23])([F:22])[F:11])[OH:6]

Participants

4

Reactant 3

HCID 11430Potassium CarbonateHCID 675612-(Trifluoromethyl)benzoyl chlorideHCID 521874O-Methylhydroxylamine hydrochloride

Product 1

HCID 20203314HCID 20203314, compound

Procedure

To a stirred solution of 25 g (0.30 mole) methoxyamine hydrochloride (NH2OCH3 :HCl) and 43 g (0.31 mole) potassium carbonate in about 200 mis ice water, 50 g (0.259 mole) of 2-trifluoromethyl-benzoylchloride were added at a slow to moderate dropping rate. The reaction mixture was stirred overnight. The mixture was suction-filtered and the residue, the crude product, was dried in a vacuum oven. The crude product was then washed with hexane (about 100 mls) and diethylether (about 2 to 3 mls), as an extra purifying step, to give the product a white solid, melting point 101° to 103° C.

Workup

  1. filtrationThe mixture was suction-filtered
  2. dry with materialthe residue, the crude product, was dried in a vacuum oven
  3. washThe crude product was then washed with hexane (about 100 mls) and diethylether (about 2 to 3 mls)
  4. customas an extra purifying step
  5. customto give the product a white solid, melting point 101° to 103° C.

Sources & evidence

ORD record
ord-e2a7a3a59e99422388f66016b2df66a6
Source dataset
uspto-grants-1984_10
Patent number
US04478832

Reaction notes

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