Phosphorus oxide (P4O10) → 24186-38-7

HRID 651587Notes

Reaction equation

HRID 651587 reaction equation
[C:1]1([CH3:12])[CH:6]=[CH:5][C:4]([CH:7]=[CH:8][C:9](Cl)=[O:10])=[CH:3][CH:2]=1.[N-:13]=[N+:14]=[N-:15].[Na+].O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O>O1CCOCC1.O.O1CCOCC1>[C:1]1([CH3:12])[CH:6]=[CH:5][C:4]([CH:7]=[CH:8][C:9]([N:13]=[N+:14]=[N-:15])=[O:10])=[CH:3][CH:2]=1

Participants

6

Reactant 3

HCID 14812Phosphorus oxide (P4O10)HCID 33557Sodium AzideHCID 53411298p-Methylcinnamoyl chloride

Product 1

HCID 5391412924186-38-7

Reagents, catalysts & solvents 2

HCID 312751,4-DioxaneSolventHCID 218864351,4-Dioxane--water (1/1)Solvent

Conditions

Temperature
7.5 °C

Procedure

3-p-Tolyl-acryloyl chloride (22.3 g, 123.3 mmol) in dioxane (50 mL) is slowly added to an ice cooled solution of sodium azide (16 g, 246.6 mmol) in water/dioxane (50 mL, 1/1, v/v) so as to maintain the temperature between 5-10° C. The mixture is stirred for 1.5 hours then poured over 300 g of ice. The resulting white solid is filtered and washed with additional water. The solid (20.72 g, 110.7 mmol) was dried over P2O5 under vacuum overnight and used in the next step without further purification.

Workup

  1. filtrationThe resulting white solid is filtered
  2. washwashed with additional water
  3. customused in the next step without further purification

Sources & evidence

ORD record
ord-2cb7e8858e39471b9809495ab6419188
Source dataset
uspto-grants-2001_08
Patent number
US06281227B1

Reaction notes

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