Phosphorus oxychloride → HCID 71679728, compound

HRID 2274960Notes

Reaction equation

HRID 2274960 reaction equation
[CH3:1][O:2][C:3]1[N:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[N:9]=[CH:8][C:7]([N+:13]([O-:15])=[O:14])=[C:6]2O.O=P(Cl)(Cl)[Cl:19]>CN(C=O)C>[Cl:19][C:6]1[C:7]([N+:13]([O-:15])=[O:14])=[CH:8][N:9]=[C:10]2[C:5]=1[N:4]=[C:3]([O:2][CH3:1])[CH:12]=[CH:11]2

Participants

4

Reactant 2

HCID 24813Phosphorus oxychlorideHCID 178487957HCID 178487957, compound

Product 1

HCID 71679728HCID 71679728, compoundYield 93%

Reagents, catalysts & solvents 1

HCID 6228DimethylformamideSolvent

Conditions

Temperature
25 °C

Procedure

The compound of Example 2 (20 g, 1 eq.) was suspended in DMF (200 mL) at 20° C. To the suspension was added POCl3 (27.7 g, 2 eq.) over a period of 15 min. The mixture was stirred at 25° C. for 35 min, poured on ice (200 g) and filtered. After drying on a rotary evaporator at 70° C., a yellow solid (20.5 g; 93% yield) was obtained.

Workup

  1. additionpoured on ice (200 g)
  2. filtrationfiltered
  3. customAfter drying on a rotary evaporator at 70° C.
  4. customa yellow solid (20.5 g; 93% yield) was obtained

Sources & evidence

ORD record
ord-936276c3b6e049c79679980575fc709a
Source dataset
uspto-grants-2015_09
Patent number
US09127002B2

Reaction notes

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