Water → Phthalic Anhydride

HRID 1707384Notes

Reaction equation

HRID 1707384 reaction equation
O.[CH:2]1[CH:7]=[C:6]([C:8]([OH:10])=O)[C:5]([C:11]([O:13]O)=[O:12])=[CH:4][CH:3]=1>CO>[C:11]1(=[O:12])[O:13][C:8](=[O:10])[C:6]2=[CH:7][CH:2]=[CH:3][CH:4]=[C:5]12

Participants

4

Reactant 2

HCID 962WaterHCID 75329Monoperoxyphthalic acid

Product 1

HCID 6811Phthalic Anhydride

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

0.81 g of 20-formamido-Δ4,17(20) -pregnadien-11β, 21-diol-3-one, 6.4 ml of water and 6.4 ml of methanol were mixed together under an inert gas atmosphere and 0.8 ml of 50% perphthalic acid (obtained from 2 g of phthalic anhydride solubilized at 40° C. over 15 minutes in a mixture of 1 ml of 50% hydrogen peroxide and 2 ml of methanol) were added with stirring at 22°-23° C. Then after 90 minutes of stirring, another 0.8 ml of perphthalic acid was added. After 4 hours, another 0.5 ml of perphthalic acid was added and after 3 hours of stirring, the mixture was cooled to 5° C. The crystals were separated and washed with water and with an aqueous solution of sodium bicarbonate and dried to obtain 0.586 g of the expected product.

Sources & evidence

ORD record
ord-42bcbb57752449d3b38b10468019b172
Source dataset
uspto-grants-1994_10
Patent number
US05352808

Reaction notes

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