p-Toluenesulfonate → p-Toluenesulfonic acid monohydrate
Reaction equation
[S:1]([C:5]1[CH:11]=[CH:10][C:8]([CH3:9])=[CH:7][CH:6]=1)([O-:4])(=[O:3])=[O:2]>O>[OH2:2].[S:1]([C:5]1[CH:11]=[CH:10][C:8]([CH3:9])=[CH:7][CH:6]=1)([OH:4])(=[O:3])=[O:2]Participants
Reactant 1
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 25 °C
Procedure
An aliquot (1.5 g, 2.2 mmol) of the tosylate anhydrous form 1 salt form of the compound of Formula I prepared above was combined with 9.0 mL of water in a sealed container for 3 days producing a scum-like material. The scum-like material was collected, broken apart, and combined with an additional 15 mL of water, producing a slurry. The slurry was shaken at 25° C. and 350 RPM for six days producing a wet cake. An additional 45 mL of water was added to the wet cake, producing a slurry, which was shaken at 25° C. and 350 RPM for five days. After the shaking period had ended the resulting solids were collected by vacuum filtration and dried under vacuum at room temperature overnight, providing the tosylate hydrate Form I salt form of the compound of Formula I.
Workup
- customproducing a scum-like material
- customThe scum-like material was collected
- customproducing a slurry
- custom350 RPM for six days producing a wet cake
- customproducing a slurry, which
- stirringwas shaken at 25° C.
- filtrationwere collected by vacuum filtration
- customdried under vacuum at room temperature overnight
Sources & evidence
- ORD record
- ord-7f779f4b81954ae88184e120bfce46b6
- Source dataset
- uspto-grants-2011_06
- Patent number
- US07956189B2
Reaction notes
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