Hydrochloric Acid → HCID 21568760, compound

HRID 1579546Notes

Reaction equation

HRID 1579546 reaction equation
[S-2:1].[Na+].[Na+].S.Cl[CH2:6][C:7]1[C:15]([Cl:16])=[C:14]([Cl:17])[C:13]([Cl:18])=[C:12]([Cl:19])[C:8]=1[C:9](Cl)=[O:10].Cl>>[Cl:16][C:15]1[C:14]([Cl:17])=[C:13]([Cl:18])[C:12]([Cl:19])=[C:8]2[C:7]=1[CH2:6][S:1][C:9]2=[O:10]

Participants

5

Reactant 4

HCID 313Hydrochloric AcidHCID 402Hydrogen SulfideHCID 14804Sodium SulfideHCID 21568761HCID 21568761, compound

Product 1

HCID 21568760HCID 21568760, compound

Conditions

Temperature
10 °C

Procedure

48 g (0.2 mole) of sodium sulfide containing water of crystallization (Na2S. 9H2O) were dissolved in 300 ml of methanol. 6.8 g (0.2 mole) of hydrogen sulfide were passed into this solution at 10° to 20°C and 32.7 g (0.1 mole) of 2-chloromethyl-3,4,5,6-tetrachlorobenzoyl chloride were then introduced at 20° to 30°C. The mixture was boiled for 6 hours under reflux and after cooling to 10°C was acidified to pH 5 with concentrated hydrochloric acid. The crystal paste which separated out was filtered off, and the residue was washed with water and acetone and dried. The yield was 27.5 g (representing 95.5% of theory) of almost colorless crystalline powder of melting point 181°-183°C.

Workup

  1. customwater of crystallization (Na2S. 9H2O)
  2. dissolutionwere dissolved in 300 ml of methanol
  3. customwere passed into this solution at 10° to 20°C
  4. temperatureunder reflux
  5. customThe crystal paste which separated out
  6. filtrationwas filtered off
  7. washthe residue was washed with water and acetone
  8. customdried

Sources & evidence

ORD record
ord-c5e3c2f2bba44997b76907d62e964ebd
Source dataset
uspto-grants-1976_01
Patent number
US03931231

Reaction notes

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