Phosphorus oxychloride → HCID 13471817, compound

HRID 2290509Notes

Reaction equation

HRID 2290509 reaction equation
O[C:2]1[N:7]2[N:8]=[C:9]([CH3:11])[CH:10]=[C:6]2[N:5]=[C:4]([CH3:12])[C:3]=1[CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH3:20].O=P(Cl)(Cl)[Cl:23]>>[Cl:23][C:2]1[N:7]2[N:8]=[C:9]([CH3:11])[CH:10]=[C:6]2[N:5]=[C:4]([CH3:12])[C:3]=1[CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH3:20]

Participants

3

Reactant 2

HCID 24813Phosphorus oxychlorideHCID 178442661HCID 178442661, compound

Product 1

HCID 13471817HCID 13471817, compound

Procedure

190 g of the condensate obtained from (a), in 550 ml of phosphorus oxytrichloride, are refluxed for 1.5 hours, after which the excess phosphorus oxytrichloride is evaporated under reduced pressure and the residue is stirred with 500 ml of CH2Cl2 and 500 ml of ice water. The organic phase is separated off, washed with three times 100 ml of ice water, dried over sodium sulfate and filtered, the solvent is evaporated under reduced pressure, and 179 g of 7-chloro-2,5-dimethyl-6-n-octylpyrazolo-[1,5-a]pyrimidine are isolated as a viscous mass.

Workup

  1. temperatureare refluxed for 1.5 hours
  2. customafter which the excess phosphorus oxytrichloride is evaporated under reduced pressure
  3. customThe organic phase is separated off
  4. washwashed with three times 100 ml of ice water
  5. dry with materialdried over sodium sulfate
  6. filtrationfiltered
  7. customthe solvent is evaporated under reduced pressure, and 179 g of 7-chloro-2,5-dimethyl-6-n-octylpyrazolo-[1,5-a]pyrimidine
  8. customare isolated as a viscous mass

Sources & evidence

ORD record
ord-580c91e744d84b1d85b92e5adad4557b
Source dataset
uspto-grants-1986_10
Patent number
US04617303

Reaction notes

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