Triethyl phosphite → HCID 14750227, compound

HRID 2073468Notes

Reaction equation

HRID 2073468 reaction equation
Cl[CH2:2][C:3]1[CH:8]=[C:7]([CH3:9])[C:6]([CH2:10][Cl:11])=[CH:5][C:4]=1[CH3:12].[CH2:13]([O:15][P:16]([O:20]CC)[O:17][CH2:18][CH3:19])[CH3:14]>>[Cl:11][CH2:10][C:6]1[CH:5]=[C:4]([CH3:12])[C:3]([CH2:2][P:16]([O:17][CH2:18][CH3:19])([O:15][CH2:13][CH3:14])=[O:20])=[CH:8][C:7]=1[CH3:9]

Participants

3

Reactant 2

HCID 31215Triethyl phosphiteHCID 80530Benzene, 1,4-bis(chloromethyl)-2,5-dimethyl-

Product 1

HCID 14750227HCID 14750227, compound

Conditions

Temperature
130 °C

Procedure

2,5-Bis(chloromethyl)-p-xylene (25 mmol) and triethylphosphite (10 mmol) were combined and heated to 130° C. under a nitrogen atmosphere for 24 hours. The reaction mixture was chromatographed on silica gel (175 gm). The column was eluted with dichloromethane until the excess starting material eluted. The eluting solvent was then changed to 5% ethanol/dichloromethane whereupon the product eluted The appropriate fractions were pooled and concentrated on a rotatory evaporator to give the product as an oil.

Workup

  1. customThe reaction mixture was chromatographed on silica gel (175 gm)
  2. washThe column was eluted with dichloromethane until the
  3. washeluted
  4. washeluted The appropriate fractions
  5. concentrationconcentrated on a rotatory evaporator

Sources & evidence

ORD record
ord-12d69d181ac64d73a7247ada15935744
Source dataset
uspto-grants-1990_04
Patent number
US04918064

Reaction notes

Loading…