Phosphorus pentachloride → HCID 19106540, compound

HRID 1197439Notes

Reaction equation

HRID 1197439 reaction equation
[CH:1]1([C:4]2[O:8][N:7]=[C:6]([C:9]3[N:10]=[CH:11][N:12]4[C:21]5[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=5)[NH:15][C:14](=O)[C:13]=34)[N:5]=2)[CH2:3][CH2:2]1.P(Cl)(Cl)(Cl)(Cl)[Cl:24]>P(Cl)(Cl)(Cl)=O>[Cl:24][C:14]1[C:13]2[N:12]([CH:11]=[N:10][C:9]=2[C:6]2[N:5]=[C:4]([CH:1]3[CH2:3][CH2:2]3)[O:8][N:7]=2)[C:21]2[C:16]([N:15]=1)=[CH:17][CH:18]=[CH:19][CH:20]=2

Participants

4

Reactant 2

HCID 24819Phosphorus pentachlorideHCID 19106542HCID 19106542, compound

Product 1

HCID 19106540HCID 19106540, compoundYield 83.9%

Reagents, catalysts & solvents 1

HCID 24813Phosphorus oxychlorideSolvent

Procedure

A ground mixture of 3-(5-cyclopropyl-1,2,4-oxadiazol-3-yl)-4,5-dihydro-4-oxo-imidazo[1,5-a]quinoxaline (3.76 g, 13 mmol) and phosphorus pentachloride (2.67 g, 13 mmol) in phosphorus oxychloride (10 ml) was stirred for 2 h at 150°-160° C. The resulting solution while still warm was poured into 200 ml of ice and stirred for 1 h. The precipitate was collected by filtration, rinsed with water and dried to give 3.4 g of the title compound, m.p. 140°-150° C. (dec.). The crude product obtained in this way was processed without further purification. (Compound 1).

Workup

  1. temperatureThe resulting solution while still warm
  2. stirringstirred for 1 h
  3. filtrationThe precipitate was collected by filtration
  4. washrinsed with water
  5. customdried

Sources & evidence

ORD record
ord-61486b9c853e40fb851c6fedf66fa8e8
Source dataset
uspto-grants-1994_01
Patent number
US05276028

Reaction notes

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