Potassium Carbonate → HCID 53902795, compound

HRID 263029Notes

Reaction equation

HRID 263029 reaction equation
C(=O)([O-])[O-].[K+].[K+].[P:7](Cl)([O:12][CH2:13][CH3:14])([O:9][CH2:10][CH3:11])=[S:8].[C:16]([C:20]1[S:21][C:22]([C:26]([O:28][CH3:29])=[O:27])=[CH:23][C:24]=1[OH:25])([O:18][CH3:19])=[O:17]>CC(C)=O>[C:16]([C:20]1[S:21][C:22]([C:26]([O:28][CH3:29])=[O:27])=[CH:23][C:24]=1[O:25][P:7]([O:12][CH2:13][CH3:14])([O:9][CH2:10][CH3:11])=[S:8])([O:18][CH3:19])=[O:17]

Participants

5

Reactant 3

HCID 11430Potassium CarbonateHCID 17305O,O-diethyl phosphorochloridothioateHCID 3056832,5-Dimethyl 3-hydroxythiophene-2,5-dicarboxylate

Product 1

HCID 53902795HCID 53902795, compoundYield 48.9%

Reagents, catalysts & solvents 1

HCID 180AcetoneSolvent

Conditions

Temperature
20 °C

Procedure

7 g of potassium carbonate and 8.9 g of O,O-diethyl chlorothiophosphate were added to a solution of 10.9 g of 2,5-dicarbomethoxy-3-hydroxy-thiophene in 500 ml of acetone and the mixture was stirred for 15 hours at 20° C. and was then filtered. The filtrate was evaporated to dryness and the residue was empasted with a 10-1 petroleum ether-isopropyl ether mixture. The mixture was vacuum filtered and the precipitate was crystallized from ethanol to obtain 8.5 g of 2,5-dicarbomethoxy-3-(diethoxythiophosphoryloxy)-thiophene melting at 50° C.

Workup

  1. filtrationwas then filtered
  2. customThe filtrate was evaporated to dryness
  3. filtrationfiltered
  4. customthe precipitate was crystallized from ethanol

Sources & evidence

ORD record
ord-83800f53ab96462dbbd0fb1bc78c67a2
Source dataset
uspto-grants-1979_05
Patent number
US04155996

Reaction notes

Loading…