Phosphorus pentachloride → HCID 570030, compound

HRID 596950Notes

Reaction equation

HRID 596950 reaction equation
P(Cl)(Cl)(Cl)(Cl)[Cl:2].O[CH2:8][S:9][C:10](=[O:17])[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1>CCOCC>[Cl:2][CH2:8][S:9][C:10](=[O:17])[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1

Participants

4

Reactant 2

HCID 24819Phosphorus pentachlorideHCID 287157S-(Hydroxymethyl) benzenecarbothioate

Product 1

HCID 570030HCID 570030, compound

Reagents, catalysts & solvents 1

HCID 3283Diethyl EtherSolvent

Procedure

42 PARTS OF PHOSPHORUS PENTACHLORIDE IS COVERED WITH A LAYER OF ABSOLUTE ETHER. While stirring and cooling with ice, an ethereal solution of 33.6 parts of hydroxymethylbenzoyl sulfide is dripped in and the whole stirred for 2 hours at room temperature. The solution is filtered, the filtrate concentrated at 0.01 mm and a bath temperature of 40° C, the residue taken up in methylene chloride and washed with cold aqueous NaNHCO3 solution. The organic phase is dried over Na2SO4 and distilled 20 parts of chloromethylbenzoyl sulfide having a boiling point at 0.1 mm of 111° to 113° C is obtained.

Workup

  1. temperaturecooling with ice
  2. stirringwhole stirred for 2 hours at room temperature
  3. filtrationThe solution is filtered
  4. concentrationthe filtrate concentrated at 0.01 mm and a bath temperature of 40° C
  5. washwashed with cold aqueous NaNHCO3 solution
  6. dry with materialThe organic phase is dried over Na2SO4
  7. distillationdistilled 20 parts of chloromethylbenzoyl sulfide having a boiling point at 0.1 mm of 111° to 113° C
  8. customis obtained

Sources & evidence

ORD record
ord-05fcd04d5e784832879799e157b6d233
Source dataset
uspto-grants-1977_03
Patent number
US04012521

Reaction notes

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