Potassium Carbonate → HCID 13339629, compound

HRID 1632126Notes

Reaction equation

HRID 1632126 reaction equation
Br[CH2:2][C:3]([CH2:12][C:13]([Cl:16])([Cl:15])[Cl:14])([C:5]1[CH:6]=[N:7][C:8]([Cl:11])=[CH:9][CH:10]=1)[OH:4].C([O-])([O-])=O.[K+].[K+]>C(#N)C>[Cl:11][C:8]1[CH:9]=[CH:10][C:5]([C:3]2([CH2:12][C:13]([Cl:16])([Cl:15])[Cl:14])[CH2:2][O:4]2)=[CH:6][N:7]=1

Participants

4

Reactant 2

HCID 11430Potassium CarbonateHCID 13339628HCID 13339628, compound

Product 1

HCID 13339629HCID 13339629, compoundYield 66%

Reagents, catalysts & solvents 1

HCID 6342AcetonitrileSolvent

Procedure

To a solution of 7.0 g (19 mmoles) of α-(bromomethyl)-6-chloro-α-(2,2,2-trichloroethyl)-3-pyridinemethanol in 200 ml of acetonitrile was added 10 g (0.07 mole) of powdered anhydrous K2CO3. The slurry was stirred for five minutes, filtered and the filtrate concentrated in vacuo, giving 5 g of crude product. Recrystallization from hexane yielded 3.6 g (66%) of product, m.p. 65°-67° C.

Workup

  1. filtrationfiltered
  2. concentrationthe filtrate concentrated in vacuo
  3. customgiving 5 g of crude product
  4. customRecrystallization from hexane

Sources & evidence

ORD record
ord-ef01ad1d3a1649efa909d004dbd0d581
Source dataset
uspto-grants-1984_10
Patent number
US04474602

Reaction notes

Loading…