Water → HCID 14303119, compound

HRID 1761384Notes

Reaction equation

HRID 1761384 reaction equation
[F:1][C:2]([F:17])([F:16])[C:3]1[CH:4]=[C:5]([CH:13]=[CH:14][CH:15]=1)[O:6][C:7]([CH3:12])([CH3:11])[C:8](=[O:10])[CH3:9].[Cl:18][CH2:19][CH2:20][CH:21](O)O.[OH2:24]>C1(C)C=CC=CC=1>[F:1][C:2]([F:16])([F:17])[C:3]1[CH:4]=[C:5]([CH:13]=[CH:14][CH:15]=1)[O:6][C:7]([C:8]1([CH3:9])[O:24][CH:20]([CH2:19][Cl:18])[CH2:21][O:10]1)([CH3:12])[CH3:11]

Participants

5

Reactant 3

HCID 962WaterHCID 14303117HCID 14303117, compoundHCID 22022801HCID 22022801, compound

Product 1

HCID 14303119HCID 14303119, compoundYield 65%

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent

Procedure

12.3 g (0.5 mol) of 3-(3-trifluoromethyl-phenoxy)-3-methyl-butan-2-one are heated under reflux together with 110 g (1 mol) of 3-chloropropanediol and 10 g of acid ion exchanger (Lewasorb A10) in 600 ml of toluene over a water separator for 14 hours. The cooled reaction mixture is filtered and the filtrate is dried over sodium sulphate and concentrated. The residue is distilled under a high vacuum. 109 g (65% of theory) of 2-[2-(3-trifluoromethyl-phenoxy)-prop-2-yl]-2-methyl-4-chloromethyl-1,3-dioxolane of boiling point 163° C. under 0.2 mbar are obtained.

Workup

  1. customThe cooled reaction mixture
  2. filtrationis filtered
  3. dry with materialthe filtrate is dried over sodium sulphate
  4. concentrationconcentrated
  5. distillationThe residue is distilled under a high vacuum

Sources & evidence

ORD record
ord-bce87a82e8434c07b8eb8a62537f59a0
Source dataset
uspto-grants-1989_05
Patent number
US04826836

Reaction notes

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