Phosphorus trichloride → 1227574-23-3

HRID 631836Notes

Reaction equation

HRID 631836 reaction equation
[Br:1][C:2]1[CH:7]=[C:6]([O:8][CH3:9])[CH:5]=[C:4]([CH3:10])[N+:3]=1[O-].P(Cl)(Cl)Cl>C(OCC)(=O)C>[Br:1][C:2]1[CH:7]=[C:6]([O:8][CH3:9])[CH:5]=[C:4]([CH3:10])[N:3]=1

Participants

4

Reactant 2

HCID 24387Phosphorus trichlorideHCID 86649695HCID 86649695, compound

Product 1

HCID 889076561227574-23-3Yield 80%

Reagents, catalysts & solvents 1

HCID 8857Ethyl AcetateSolvent

Procedure

2-Bromo-6-methyl-4-methoxy-pyridine 1-oxide (3.3 g, 15 mmol) was dissolved in ethyl acetate (anhydrous, 100 ml), phosphorus trichloride (6.6 ml) was added dropwise and the mixture was stirred at room temperature for three hours. The precipitate was collected by filtration, washed with ethyl acetate and dried to yield 2.4 g of beige crystals (12 mmol, 79%) MS(APCI) m/z=203.9 [M+1]+.

Workup

  1. filtrationThe precipitate was collected by filtration
  2. washwashed with ethyl acetate
  3. customdried

Sources & evidence

ORD record
ord-b959dd7b968445b8ae2898790144d1b0
Source dataset
uspto-grants-2016_04
Patent number
US09321724B2

Reaction notes

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