Phosphorus oxychloride → HCID 86046565, compound

HRID 1626317Notes

Reaction equation

HRID 1626317 reaction equation
[C:1]1([C:7]2[N:8]([C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=3)[C:9]3[N:10]=[CH:11][NH:12][C:13](=O)[C:14]=3[N:15]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.O=P(Cl)(Cl)[Cl:25]>>[Cl:25][C:13]1[N:12]=[CH:11][N:10]=[C:9]2[C:14]=1[N:15]=[C:7]([C:1]1[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1)[N:8]2[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1

Participants

3

Reactant 2

HCID 24813Phosphorus oxychlorideHCID 136410984HCID 136410984, compound

Product 1

HCID 86046565HCID 86046565, compoundYield 84%

Conditions

Temperature
110 °C

Procedure

8,9-diphenyl-1H-purin-6(9H)-one obtained in step 3 (22.3 g, 77.4 mmol) was dissolved in POCl3 (70 ml) at 0° C. and the reaction mixture was heated to reflux at 110° C. overnight. After cooled to room temperature, ice-water was added to the resulting reaction mixture and stirred for 30 min at room temperature. The resulting mixture was filtered with water. The collected solid was dried under reduced pressure to obtain the title compound (20 g, 84%) as beige solid.

Workup

  1. temperaturethe reaction mixture was heated
  2. temperatureAfter cooled to room temperature
  3. filtrationThe resulting mixture was filtered with water
  4. customThe collected solid was dried under reduced pressure

Sources & evidence

ORD record
ord-4f4e4e4412884e44a1beb83d1b1fbe15
Source dataset
uspto-grants-2014_07
Patent number
US08785453B2

Reaction notes

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