Triethylamine → HCID 12585423, compound

HRID 1643324Notes

Reaction equation

HRID 1643324 reaction equation
C(N(CC)CC)C.[CH3:8][O:9][C:10]1[CH:15]=[CH:14][C:13]([OH:16])=[CH:12][CH:11]=1.[P:17](Cl)([Cl:20])([Cl:19])=[O:18]>CCOCC>[P:17]([Cl:20])([Cl:19])(=[O:18])[O:16][C:13]1[CH:14]=[CH:15][C:10]([O:9][CH3:8])=[CH:11][CH:12]=1

Participants

5

Reactant 3

HCID 8471TriethylamineHCID 90154-MethoxyphenolHCID 24813Phosphorus oxychloride

Product 1

HCID 12585423HCID 12585423, compoundYield 92%

Reagents, catalysts & solvents 1

HCID 3283Diethyl EtherSolvent2×

Procedure

Dry triethylamine (4.2 ml, 30 mmol) and p-methoxyphenol (3.72 g, 30 mmol) in 100 ml dry ether were added dropwise to a stirred solution of dry ether (50 ml) containing phosphorus oxychloride (2.80 ml, 30 mmol), at −78° C. under nitrogen. Following the addition, the reaction mixture was slowly allowed to warm at room temperature and stirred for one hour. The solvent was removed under reduced pressure to give the crude product (6.6 g, 92%) as an oil, which was used in the following step without any further purification.

Workup

  1. customat −78° C.
  2. additionthe addition
  3. customThe solvent was removed under reduced pressure

Sources & evidence

ORD record
ord-8cbafd57609f4b7091c5360240351ed3
Source dataset
uspto-grants-2012_02
Patent number
US08119779B2

Reaction notes

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