Triethylamine → HCID 18402791, compound

HRID 861838Notes

Reaction equation

HRID 861838 reaction equation
[OH:1][C:2]([C:11]1[CH:16]=[CH:15][CH:14]=[C:13]([C:17]([C:23]([F:26])([F:25])[F:24])([OH:22])[C:18]([F:21])([F:20])[F:19])[CH:12]=1)([C:7]([F:10])([F:9])[F:8])[C:3]([F:6])([F:5])[F:4].C(N(CC)CC)C.[CH3:34][S:35](Cl)(=[O:37])=[O:36]>C(Cl)Cl>[CH3:34][S:35]([O:22][C:17]([C:13]1[CH:14]=[CH:15][CH:16]=[C:11]([C:2]([C:3]([F:6])([F:5])[F:4])([O:1][S:35]([CH3:34])(=[O:37])=[O:36])[C:7]([F:10])([F:9])[F:8])[CH:12]=1)([C:18]([F:19])([F:20])[F:21])[C:23]([F:24])([F:25])[F:26])(=[O:37])=[O:36]

Participants

5

Reactant 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 699331,3-Benzenedimethanol, .alpha.1,.alpha.1,.alpha.3,.alpha.3-tetrakis(trifluoromethyl)-

Product 1

HCID 18402791HCID 18402791, compoundYield 98.9%

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

4.1 g (10 mmol) of 1,3-bis-(1-hydroxy-1-trifluoromethyl-2,2,2-trifluoroethyl)-benzene were dissolved in 50 ml of methylene chloride, and 2.5 g (25 mmol) of triethylamine were added. 3.64 g (25 mmol) of methanesulfonyl chloride were then added dropwise. The mixture was stirred for 8 hours at room temperature, separated off from the precipitated salt and evaporated down. 5.6 g of 1,3-bis-(1-methanesulfonyloxy-1-trifluoromethyl-2,2,2-trifluoro-ethyl)-benzene were obtained (colorless crystals, m.p.: 125° C. [from diisopropyl diether]).

Workup

  1. customseparated off from the precipitated salt
  2. customevaporated down

Sources & evidence

ORD record
ord-5b18020184714fa68ca55232a1062d6c
Source dataset
uspto-grants-1998_02
Patent number
US05716756

Reaction notes

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