Dimethyl methylphosphonate → HCID 22916487, compound

HRID 259702Notes

Reaction equation

HRID 259702 reaction equation
[Cl:1][C:2]1[C:3]([C:7]2[CH:12]=[CH:11][CH:10]=[C:9]([Cl:13])[C:8]=2[Cl:14])=[N:4][NH:5][CH:6]=1.[CH3:15]P(=O)(OC)OC.C([O-])(O)=O.[Na+]>>[CH3:15][N:5]1[CH:6]=[C:2]([Cl:1])[C:3]([C:7]2[CH:12]=[CH:11][CH:10]=[C:9]([Cl:13])[C:8]=2[Cl:14])=[N:4]1

Participants

4

Reactant 3

HCID 12958Dimethyl methylphosphonateHCID 516892Sodium BicarbonateHCID 178478290HCID 178478290, compound

Product 1

HCID 22916487HCID 22916487, compound

Procedure

1.5 g of 4-chloro-3-(2,3-dichlorophenyl)pyrazole and 0.40 g of dimethyl methylphosphonate are heated at 150° C. for 1 hour. After returning to room temperature, the mixture is taken up in a saturated aqueous NaHCO3 solution and extracted with 2×50 ml of CH2Cl2. The combined organic phases are dried over Na2SO4 and concentrated under reduced pressure. The crude solid is purified by liquid chromatography on a silica column (eluent: heptane/ethyl acetate [80/20]).

Workup

  1. customAfter returning to room temperature
  2. extractionextracted with 2×50 ml of CH2Cl2
  3. dry with materialThe combined organic phases are dried over Na2SO4
  4. concentrationconcentrated under reduced pressure
  5. customThe crude solid is purified by liquid chromatography on a silica column (eluent: heptane/ethyl acetate [80/20])

Sources & evidence

ORD record
ord-f2caf968e2af4f0c90a100912641fa33
Source dataset
uspto-grants-1996_06
Patent number
US05523280

Reaction notes

Loading…