Diethyl Ether → HCID 12495482, compound

HRID 1704640Notes

Reaction equation

HRID 1704640 reaction equation
[C:1]1([N:7]2[C:11](=O)[CH:10]=[N:9][S:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.CCOCC.P(Cl)(Cl)([Cl:20])=O>>[Cl-:20].[C:1]1([N+:7]2[S:8][N:9]=[CH:10][C:11]=2[Cl:20])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

Participants

4

Reactant 3

HCID 3283Diethyl EtherHCID 24813Phosphorus oxychlorideHCID 12495460HCID 12495460, compound

Product 1

HCID 12495482HCID 12495482, compound

Procedure

2-Phenyl-1,2,5-thiadiazole-3-one (3.1 g., 0.02 mole) was refluxed for 4 minutes in phosphorus oxychloride (20 ml.) and then cooled slowly. Ether (60-100 ml.) was added and the precipitate was filtered in a stream of nitrogen and washed well with anhydrous ether. The precipitate was then triturated with acetonitrile, refiltered and rewashed with acetonitrile and dried in a stream of nitrogen, m.p. (dec.) 110° C.

Workup

  1. temperaturecooled slowly
  2. filtrationthe precipitate was filtered in a stream of nitrogen
  3. washwashed well with anhydrous ether
  4. customThe precipitate was then triturated with acetonitrile
  5. customdried in a stream of nitrogen
  6. custom(dec.) 110° C.

Sources & evidence

ORD record
ord-0d9061254d7c4ee18755c6dd4c2cd480
Source dataset
uspto-grants-1978_11
Patent number
US04127584

Reaction notes

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