【药物名称】Indobufen, K-3920, Ibustrin
化学结构式(Chemical Structure):
参考文献No.53559
标题:Indobufen
作者:de Angelis, L.; Casta馿r, J.
来源:Drugs Fut 1979,4(2),109
合成路线图解说明:

The reaction of phthalic anhydride (I) with ethyl p-amino-alpha-ethylphenylacetate (II) in refluxing acetic acid gives ethyl alpha-[4-(1,3-dioxo-2-isoindolinyl)phenyl]-n-butyrate (III), which is reduced with Zn in refluxing acetic acid to the isoindolinone (IV). Finally, this compound is hydrolyzed with K2CO3 in refluxing ethanol - water.

合成路线图解说明:

The reaction of (II) with phthalide (V) at 280 C gives the isoindolinone (IV). Finally, this compound is hydrolyzed with K2CO3 in refluxing ethanol - water.

合成路线图解说明:

The reaction of (II) with benzaldehyde (VI) in refluxing toluene gives ethyl p-benzylideneamino-alpha-methylphenylacetate (VII), which is reduced with H2 over PtO2 in ethanol to the N-benzyl derivative (VIII). The acylation of (VIII) with phosgene by means of pyridine in toluene yields the N-chlorocarbonyl compound (IX), which is then cyclized to the isoindolinone (IV) with AlCl3 in refluxing 1,2-dichloroethane. Finally, this compound is hydrolyzed with K2CO3 in refluxing ethanol - water.

合成路线图解说明:

By cyclization of phthalic aldehyde with p-amino-8-ethylphenylacetic acid (XI) in DMF at 100 C.

合成路线图解说明:

The cyclization of (XI) with o-cyanobenzyl bromide (XII) in refluxing ethanol gives 1-imino-2-[p-[(alpha-ethyl)carboxymethyl]phenyl]isoindoline (XIII), which is finally hydrolyzed with K2CO3 in refluxing ethanol water.

合成路线图解说明:

The reaction of benzaldehyde (VI) with p-amino-alpha-ethylphenylacetonitrile (XIV) in refluxing toluene gives p-benzylideneamino-alpha-ethylphenylacetonitrile (XV), which is reduced with H2 over PtO2 in ethanol yielding p-benzylamino-alpha-ethylphenylacetonitrile (XVI). The acylation of (XVI) with phosgene by means of pyridine in toluene affords the N-chlorocarbo-nyl compound (XVII), which is cyclized with AlCl3 in refluxing 1,2-dichloroethane to yield 1-oxo-2-[p-(alpha-ethyl-cyanomethyl)phenyl]isoindoline (XVIII). Finally, this compound is hydrolyzed with H2SO4 in refluxing water.

参考文献No.604468
标题:New analgesic-antiinflammatory drugs. 1-oxo-2-substituted isoindoline derivatives
作者:Nannini, G.; et al.
来源:Arzneim-Forsch Drug Res 1973,23(8),1090
合成路线图解说明:

The reaction of phthalic anhydride (I) with ethyl p-amino-alpha-ethylphenylacetate (II) in refluxing acetic acid gives ethyl alpha-[4-(1,3-dioxo-2-isoindolinyl)phenyl]-n-butyrate (III), which is reduced with Zn in refluxing acetic acid to the isoindolinone (IV). Finally, this compound is hydrolyzed with K2CO3 in refluxing ethanol - water.

合成路线图解说明:

The reaction of (II) with benzaldehyde (VI) in refluxing toluene gives ethyl p-benzylideneamino-alpha-methylphenylacetate (VII), which is reduced with H2 over PtO2 in ethanol to the N-benzyl derivative (VIII). The acylation of (VIII) with phosgene by means of pyridine in toluene yields the N-chlorocarbonyl compound (IX), which is then cyclized to the isoindolinone (IV) with AlCl3 in refluxing 1,2-dichloroethane. Finally, this compound is hydrolyzed with K2CO3 in refluxing ethanol - water.

合成路线图解说明:

The cyclization of (XI) with o-cyanobenzyl bromide (XII) in refluxing ethanol gives 1-imino-2-[p-[(alpha-ethyl)carboxymethyl]phenyl]isoindoline (XIII), which is finally hydrolyzed with K2CO3 in refluxing ethanol water.

参考文献No.700952
标题:D閞iv閟 d'iso-indoline et proc閐?de leur pr閜aration
作者:Giraldi, P.N.; et al.
来源:DE 2154525; FR 2112480; JP 51068563; JP 52017463; NL 7115288
合成路线图解说明:

The reaction of phthalic anhydride (I) with ethyl p-amino-alpha-ethylphenylacetate (II) in refluxing acetic acid gives ethyl alpha-[4-(1,3-dioxo-2-isoindolinyl)phenyl]-n-butyrate (III), which is reduced with Zn in refluxing acetic acid to the isoindolinone (IV). Finally, this compound is hydrolyzed with K2CO3 in refluxing ethanol - water.

合成路线图解说明:

The reaction of (II) with phthalide (V) at 280 C gives the isoindolinone (IV). Finally, this compound is hydrolyzed with K2CO3 in refluxing ethanol - water.

合成路线图解说明:

By cyclization of phthalic aldehyde with p-amino-8-ethylphenylacetic acid (XI) in DMF at 100 C.

合成路线图解说明:

The cyclization of (XI) with o-cyanobenzyl bromide (XII) in refluxing ethanol gives 1-imino-2-[p-[(alpha-ethyl)carboxymethyl]phenyl]isoindoline (XIII), which is finally hydrolyzed with K2CO3 in refluxing ethanol water.

参考文献No.700953
标题:Verfahren zur Herstellung von Isoindolinderivaten
作者:Giraldi, P.N.; et al.
来源:AT 325604B; CA 994785; CH 581106; JP 48057965; NL 7215830
合成路线图解说明:

The reaction of (II) with benzaldehyde (VI) in refluxing toluene gives ethyl p-benzylideneamino-alpha-methylphenylacetate (VII), which is reduced with H2 over PtO2 in ethanol to the N-benzyl derivative (VIII). The acylation of (VIII) with phosgene by means of pyridine in toluene yields the N-chlorocarbonyl compound (IX), which is then cyclized to the isoindolinone (IV) with AlCl3 in refluxing 1,2-dichloroethane. Finally, this compound is hydrolyzed with K2CO3 in refluxing ethanol - water.

合成路线图解说明:

The reaction of benzaldehyde (VI) with p-amino-alpha-ethylphenylacetonitrile (XIV) in refluxing toluene gives p-benzylideneamino-alpha-ethylphenylacetonitrile (XV), which is reduced with H2 over PtO2 in ethanol yielding p-benzylamino-alpha-ethylphenylacetonitrile (XVI). The acylation of (XVI) with phosgene by means of pyridine in toluene affords the N-chlorocarbo-nyl compound (XVII), which is cyclized with AlCl3 in refluxing 1,2-dichloroethane to yield 1-oxo-2-[p-(alpha-ethyl-cyanomethyl)phenyl]isoindoline (XVIII). Finally, this compound is hydrolyzed with H2SO4 in refluxing water.

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