Triethylamine → HCID 53844714, compound

HRID 1649560Notes

Reaction equation

HRID 1649560 reaction equation
C(N(CC)CC)C.[CH3:8][N:9]([C:13]([Cl:16])([Cl:15])[Cl:14])[C:10](F)=[S:11].[CH3:17][N:18]1[CH:22]=[C:21]([OH:23])[CH:20]=[N:19]1>C1(C)C=CC=CC=1>[CH3:17][N:18]1[CH:22]=[C:21]([O:23][C:10](=[S:11])[N:9]([CH3:8])[C:13]([Cl:16])([Cl:15])[Cl:14])[CH:20]=[N:19]1

Participants

5

Reactant 3

HCID 8471TriethylamineHCID 130184091-Methyl-1H-pyrazol-4-olHCID 54242865HCID 54242865, compound

Product 1

HCID 53844714HCID 53844714, compoundYield 86.6%

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent

Procedure

5.1 g (0.05 mol) of triethylamine were added dropwise to a mixture of 11.3 g (0.05 mol) of N-methyl-N-trichloromethylthio-carbamoyl fluoride, 4.9 g (0.05 mol) of 1-methyl-4-hydroxypyrazole and 150 ml of toluene. After 4 hours, the mixture was extracted twice with 25 ml of water each time. The organic phase was dried over sodium sulphate and evaporated in vacuo. The residue was subjected to incipient distillation under a high vacuum. 12.5 g (82% of theory) of N-methyl-N-trichloromethylthiocarbamic acid O-(1-methyl-pyrazol-4-yl) ester were thus obtained in the form of a yellow oil with a refractive index nD23 of 1.5492.

Workup

  1. extractionthe mixture was extracted twice with 25 ml of water each time
  2. dry with materialThe organic phase was dried over sodium sulphate
  3. customevaporated in vacuo
  4. distillationThe residue was subjected to incipient distillation under a high vacuum

Sources & evidence

ORD record
ord-3a8bd01653cd4bc3b53a9023fef2ece7
Source dataset
uspto-grants-1983_11
Patent number
US04418073

Reaction notes

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