p-Toluenesulfonic acid monohydrate → p-Toluenesulfonic acid

HRID 1105760Notes

Reaction equation

HRID 1105760 reaction equation
O.[C:2]1([CH3:12])[CH:7]=[CH:6][C:5]([S:8]([OH:11])(=[O:10])=[O:9])=[CH:4][CH:3]=1>O>[C:2]1([CH3:12])[CH:3]=[CH:4][C:5]([S:8]([OH:11])(=[O:9])=[O:10])=[CH:6][CH:7]=1

Participants

3

Reactant 1

HCID 521998p-Toluenesulfonic acid monohydrate

Product 1

HCID 6101p-Toluenesulfonic acid

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Conditions

Temperature
115 °C

Procedure

To a 12 liter, 4-neck round bottom flask was added 9,072 g p-toluene sulfonic acid monohydrate which was heated under a nitrogen atmosphere to 115° C. The pressure was reduced to 220 mm and reduced further to 20 mm over the next 1.5 hours. The contents were held at 115°-117° C./22 mm for a total of 14 hours to obtain the theoretical amount of water. The molten anhydrous acid was packaged in 16 oz. plastic jars and purged with nitrogen before sealing with a tight cap.

Workup

  1. customreduced further to 20 mm over the next 1.5 hours
  2. customwere held at 115°-117° C.
  3. customfor a total of 14 hours
  4. custompurged with nitrogen

Sources & evidence

ORD record
ord-4a41e9fb48044fe6bf37e637d1a22c31
Source dataset
uspto-grants-1982_01
Patent number
US04310426

Reaction notes

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