dimethyl 4-dimethylaminophthalate synthesis
- Product Name:dimethyl 4-dimethylaminophthalate
- CAS Number:39617-05-5
- Molecular formula:C12H15NO4
- Molecular Weight:237.2518
610-22-0
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Yield:39617-05-5 85%
Reaction Conditions:
with formaldehyd;propionic acid;aluminum nickel in methanol;water;
Steps:
11 4-dimethylamino-phthalic acid dimethyl ester
EXAMPLE 11 4-dimethylamino-phthalic acid dimethyl ester 90 parts of 4-nitrophthalic acid dimethyl ester are suspended in 580 parts of methanol and are hydrogenated at 60° C under 100 atmospheres hydrogen pressure, after addition of 90 parts of aqueous formaldehyde solution (40 per cent strength), 18 parts of propionic acid and 9 parts of Raney nickel. After the hydrogen uptake has ceased, the mixture is freed from the catalyst by filtration and the methanolic solution is diluted with 2,000 parts of water. 4-dimethylaminophthalic acid dimethyl ester separates out initially as an oil, which is separated off and crystallizes to colorless crystals. 75 parts of 4-dimethylamino-phthalic acid dimethyl ester of melting point 54° to 57° C are obtained, corresponding to a yield of 85% of theory.
References:
US4002664,1977,A
