Phosphorus trichloride → HCID 59804967, compound

HRID 604850Notes

Reaction equation

HRID 604850 reaction equation
O[C:2]1[N:7]=[C:6]([C:8]2[CH:9]=[C:10]([P:14]([C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=3)[C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=3)[CH:11]=[CH:12][CH:13]=2)[CH:5]=[CH:4][N:3]=1.P(Cl)(Cl)[Cl:28]>C(Cl)(Cl)Cl>[Cl:28][C:2]1[N:7]=[C:6]([C:8]2[CH:9]=[C:10]([P:14]([C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=3)[C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=3)[CH:11]=[CH:12][CH:13]=2)[CH:5]=[CH:4][N:3]=1

Participants

4

Reactant 2

HCID 24387Phosphorus trichlorideHCID 178517731HCID 178517731, compound

Product 1

HCID 59804967HCID 59804967, compoundYield 90%

Reagents, catalysts & solvents 1

HCID 6212ChloroformSolvent

Procedure

5 mmol of 20 are dissolved in 50 ml of CHCl3 and mixed with 10 mmol of PCl3. It is refluxed for 30 min, the volatiles are removed in a vacuum and the colorless solid is washed with water. Recrystallization from chloroform gives 21 in a yield above 90%. ESI MS, m/z (%): 375.8154 (100) [M+H]+. 31P{1H} NMR (101.2 MHz, 25° C., DMSO-d6): δ −7.40.

Workup

  1. temperatureIt is refluxed for 30 min
  2. customthe volatiles are removed in a vacuum
  3. washthe colorless solid is washed with water
  4. customRecrystallization from chloroform

Sources & evidence

ORD record
ord-ec13db15f31445948c272cba2deaa9a4
Source dataset
uspto-grants-2011_03
Patent number
US07910744B2

Reaction notes

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