Phosgene → HCID 15285934, compound

HRID 260058Notes

Reaction equation

HRID 260058 reaction equation
[F:1][C:2]([F:18])([F:17])[CH2:3][CH2:4][CH2:5][O:6][C:7]1[CH:16]=[CH:15][C:10]([C:11]([NH:13][NH2:14])=[O:12])=[CH:9][CH:8]=1.[C:19](Cl)(Cl)=[O:20]>C1(C)C=CC=CC=1>[F:1][C:2]([F:17])([F:18])[CH2:3][CH2:4][CH2:5][O:6][C:7]1[CH:16]=[CH:15][C:10]([C:11]2[O:12][C:19](=[O:20])[NH:14][N:13]=2)=[CH:9][CH:8]=1

Participants

4

Reactant 2

HCID 6371Phosgene2×HCID 15285932HCID 15285932, compound

Product 1

HCID 15285934HCID 15285934, compound

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent2×

Procedure

4.09 g of 4-(4,4,4-trifluorobutoxy)benzoic acid hydrazide, dissolved in 56 ml of hot toluene, are introduced into a 100 ml three-necked flask under nitrogen at room temperature. 12.1 ml of phosgene dissolved in toluene (1.93M) are then added dropwise. The mixture is heated to 100°-110° C. for 1 h 30 min and the excess phosgene is then stripped off using a stream of nitrogen. The reaction medium is cooled and the precipitate formed is filtered off and dried under vacuum. 4.4 g of product are obtained.

Workup

  1. additionare introduced into a 100 ml three-necked flask under nitrogen at room temperature
  2. additionare then added dropwise
  3. temperatureThe mixture is heated to 100°-110° C. for 1 h 30 min
  4. temperatureThe reaction medium is cooled
  5. customthe precipitate formed
  6. filtrationis filtered off
  7. customdried under vacuum

Sources & evidence

ORD record
ord-5f107f24948a46bda02ee5267364a825
Source dataset
uspto-grants-1996_06
Patent number
US05525619

Reaction notes

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