Potassium Carbonate → HCID 20357800, compound

HRID 1658010Notes

Reaction equation

HRID 1658010 reaction equation
[CH:1]([NH:3][CH:4](P(OCC)(OCC)=O)[C:5]([O:7][CH2:8][C:9]([Cl:12])([Cl:11])[Cl:10])=[O:6])=[S:2].C(=O)([O-])[O-].[K+].[K+].Cl[CH2:28][C:29](=O)[CH2:30][O:31][CH2:32][O:33][CH3:34]>CC(C)=O.C(Cl)Cl>[CH3:34][O:33][CH2:32][O:31][CH2:30][C:29]1[CH2:28][S:2][CH:1]=[N:3][C:4]=1[C:5]([O:7][CH2:8][C:9]([Cl:10])([Cl:11])[Cl:12])=[O:6]

Participants

6

Reactant 3

HCID 11430Potassium CarbonateHCID 203578282-Propanone, 1-chloro-3-(methoxymethoxy)-HCID 86733535HCID 86733535, compound

Product 1

HCID 20357800HCID 20357800, compound

Reagents, catalysts & solvents 2

HCID 180AcetoneSolventHCID 6344DichloromethaneSolvent

Procedure

A solution of 2,2,2-trichloroethyl α-thioformamidodiethylphosphonoacetate (3.87 g.) in acetone (50 ml.) is treated with powdered potassium carbonate (4.15 g) and 1-chloro-3-methoxymethyloxy-propan-2-one (1.60 g.). The mixture is stirred for 4 hrs. at room temperature under a nitrogen atmosphere, then filtered. Evaporation of the filtrate leaves a residue which is dissolved in methylene chloride. The solution is washed with dilute aqueous dipotassium hydrogen phosphate and water, dried over magnesium sulfate, filtered and evaporated in vacuo affording 2,2,2-trichloroethyl 5-methoxymethyloxymethyl-6H-1,3-thiazine-4-carboxylate.

Workup

  1. filtrationat room temperature under a nitrogen atmosphere, then filtered
  2. customEvaporation of the filtrate
  3. customleaves a residue which
  4. washThe solution is washed with dilute aqueous dipotassium hydrogen phosphate and water
  5. dry with materialdried over magnesium sulfate
  6. filtrationfiltered
  7. customevaporated in vacuo

Sources & evidence

ORD record
ord-70e84ea1a45b44079d428ca3c41cfd11
Source dataset
uspto-grants-1976_06
Patent number
US03962224

Reaction notes

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