Hydrochloric Acid → HCID 13799281, compound

HRID 652313Notes

Reaction equation

HRID 652313 reaction equation
[C:1](OC(=O)C)(=[O:3])[CH3:2].[CH3:8][O:9][C:10]1[CH:15]=[CH:14][CH:13]=[C:12]([O:16][CH3:17])[C:11]=1[CH:18]([OH:26])[C:19]([Cl:25])([Cl:24])[C:20]([F:23])([F:22])[F:21].N1C=CC=CC=1.Cl>>[CH3:8][O:9][C:10]1[CH:15]=[CH:14][CH:13]=[C:12]([O:16][CH3:17])[C:11]=1[CH:18]([O:26][C:1](=[O:3])[CH3:2])[C:19]([Cl:25])([Cl:24])[C:20]([F:21])([F:22])[F:23]

Participants

5

Reactant 4

HCID 313Hydrochloric AcidHCID 1049PyridineHCID 7918Acetic AnhydrideHCID 13799280HCID 13799280, compound

Product 1

HCID 13799281HCID 13799281, compoundYield 87%

Procedure

31 ml (0.33 mole) of acetic anhydride are added to 97.6 g (0.30 mole) of 1,3-dimethoxy-2-(1-hydroxy-2,2-dichloro-3,3,3-trifluoro-propyl)-benzene in a 500 ml pear-shaped flask at room temperature. 30 ml (0.36 mole) of pyridine are then added to the dark red solution (weakly exothermic). The reaction solution is stirred at room temperature for 3 days. The reaction mixture is then poured onto ice and acidified with 10% hydrochloric acid. It is extracted with ether and the extract is washed with water and brine, dried over magnesium sulfate and evaporated to dryness. The 1,3-dimethoxy-2-(1-acetoxy-2,2-dichloro-3,3,3-trifluoropropyl)-benzene which remains (yield 87%) is employed for stage D without further purification.

Workup

  1. additionThe reaction mixture is then poured onto ice
  2. extractionIt is extracted with ether
  3. washthe extract is washed with water and brine
  4. dry with materialdried over magnesium sulfate
  5. customevaporated to dryness
  6. customis employed for stage D without further purification

Sources & evidence

ORD record
ord-05df195ff0dc4278b9999b49062beb95
Source dataset
uspto-grants-1987_06
Patent number
US04670604

Reaction notes

Loading…