Phosphorus oxychloride → HCID 11637267, compound

HRID 1986637Notes

Reaction equation

HRID 1986637 reaction equation
[CH3:1][C:2]1[C:7]([CH:8]2[CH2:12][CH2:11][CH2:10][CH2:9]2)=[C:6](O)[N:5]2[N:14]=[CH:15][N:16]=[C:4]2[N:3]=1.O=P(Cl)(Cl)[Cl:19]>>[CH3:1][C:2]1[C:7]([CH:8]2[CH2:12][CH2:11][CH2:10][CH2:9]2)=[C:6]([Cl:19])[N:5]2[N:14]=[CH:15][N:16]=[C:4]2[N:3]=1

Participants

3

Reactant 2

HCID 24813Phosphorus oxychlorideHCID 178432402HCID 178432402, compound

Product 1

HCID 11637267HCID 11637267, compound

Procedure

A mixture of 5-methyl-6-cyclopentyl-7-hydroxy[1,2,4]triazolo[1,5-a]pyrimidine (17 g, Ex. 2) and POCl3 (50 ml) was heated under reflux for 8 hours. During this operation, some of the POCl3 was distilled off. The residue was poured into a mixture of dichloromethane and water. The organic phase was separated off and dried. Removal of the solvent gave 11 g of the title compound of m.p. 87° C.

Workup

  1. temperaturewas heated
  2. temperatureunder reflux for 8 hours
  3. distillationDuring this operation, some of the POCl3 was distilled off
  4. additionThe residue was poured into a mixture of dichloromethane and water
  5. customThe organic phase was separated off
  6. customdried
  7. customRemoval of the solvent

Sources & evidence

ORD record
ord-90a1eb9386714ac5b38c7442dba9946b
Source dataset
uspto-grants-2009_06
Patent number
US07550471B2

Reaction notes

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