Ethyl chloroformate → HCID 13020003, compound

HRID 1277830Notes

Reaction equation

HRID 1277830 reaction equation
[F:1][C:2]([F:18])([F:17])[C:3]1[CH:4]=[C:5]([CH:14]=[CH:15][CH:16]=1)[O:6][C:7]1[CH:12]=[CH:11][C:10]([NH2:13])=[CH:9][CH:8]=1.Cl[C:20]([O:22][CH2:23][CH3:24])=[O:21]>N1C=CC=CC=1>[F:1][C:2]([F:17])([F:18])[C:3]1[CH:4]=[C:5]([CH:14]=[CH:15][CH:16]=1)[O:6][C:7]1[CH:8]=[CH:9][C:10]([NH:13][C:20](=[O:21])[O:22][CH2:23][CH3:24])=[CH:11][CH:12]=1

Participants

4

Reactant 2

HCID 10928Ethyl chloroformateHCID 27607504-[3-(trifluoromethyl)phenoxy]aniline

Product 1

HCID 13020003HCID 13020003, compound

Reagents, catalysts & solvents 1

HCID 1049PyridineSolvent

Procedure

4-[3-(trifluoromethyl)phenoxy]benzenamine (6.0 grams; 0.21 mol) and pyridine (50 ml) were placed in a glass reaction vessel equipped with a mechanical stirrer and placed in an ice bath. Ethyl chloroformate (5 ml) was added dropwise to the reaction mixture with continuous stirring. Stirring was continued overnight and the mixture was then poured into ice water (500 ml). The precipitate was washed with water and dried. It was found to have a melting point of 74°-75.5° C. In fraud analysis confirmed the identity of the desired product.

Workup

  1. customequipped with a mechanical stirrer
  2. customplaced in an ice bath
  3. washThe precipitate was washed with water
  4. customdried

Sources & evidence

ORD record
ord-4dd1c15ce9b9459bbf8b89c9e685a1cf
Source dataset
uspto-grants-1981_07
Patent number
US04279637

Reaction notes

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