RO81056B - Process for preparing n-(3-(1', 3'-oxapenthiamethylenaminoethylidenamino)2, 4, 6-triiodinebenzoyl)-beta-amino-alpha methylpropionic acid - Google Patents
Process for preparing n-(3-(1', 3'-oxapenthiamethylenaminoethylidenamino)2, 4, 6-triiodinebenzoyl)-beta-amino-alpha methylpropionic acidInfo
- Publication number
- RO81056B RO81056B RO103041A RO10304180A RO81056B RO 81056 B RO81056 B RO 81056B RO 103041 A RO103041 A RO 103041A RO 10304180 A RO10304180 A RO 10304180A RO 81056 B RO81056 B RO 81056B
- Authority
- RO
- Romania
- Prior art keywords
- molar equivalents
- beta
- alpha
- amino
- methylpropionic acid
- Prior art date
Links
- 238000004519 manufacturing process Methods 0.000 title 1
- 238000000034 method Methods 0.000 abstract 2
- 150000002825 nitriles Chemical class 0.000 abstract 2
- KYWXRBNOYGGPIZ-UHFFFAOYSA-N 1-morpholin-4-ylethanone Chemical compound CC(=O)N1CCOCC1 KYWXRBNOYGGPIZ-UHFFFAOYSA-N 0.000 abstract 1
- 239000002253 acid Substances 0.000 abstract 1
- 239000003929 acidic solution Substances 0.000 abstract 1
- 238000009835 boiling Methods 0.000 abstract 1
- 238000001704 evaporation Methods 0.000 abstract 1
- 230000008020 evaporation Effects 0.000 abstract 1
- XHXFXVLFKHQFAL-UHFFFAOYSA-N phosphoryl trichloride Chemical compound ClP(Cl)(Cl)=O XHXFXVLFKHQFAL-UHFFFAOYSA-N 0.000 abstract 1
- 230000001376 precipitating effect Effects 0.000 abstract 1
- 238000002360 preparation method Methods 0.000 abstract 1
- 239000000376 reactant Substances 0.000 abstract 1
- 239000011541 reaction mixture Substances 0.000 abstract 1
- 239000002904 solvent Substances 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D295/00—Heterocyclic compounds containing polymethylene-imine rings with at least five ring members, 3-azabicyclo [3.2.2] nonane, piperazine, morpholine or thiomorpholine rings, having only hydrogen atoms directly attached to the ring carbon atoms
- C07D295/16—Heterocyclic compounds containing polymethylene-imine rings with at least five ring members, 3-azabicyclo [3.2.2] nonane, piperazine, morpholine or thiomorpholine rings, having only hydrogen atoms directly attached to the ring carbon atoms acylated on ring nitrogen atoms
- C07D295/18—Heterocyclic compounds containing polymethylene-imine rings with at least five ring members, 3-azabicyclo [3.2.2] nonane, piperazine, morpholine or thiomorpholine rings, having only hydrogen atoms directly attached to the ring carbon atoms acylated on ring nitrogen atoms by radicals derived from carboxylic acids, or sulfur or nitrogen analogues thereof
- C07D295/195—Radicals derived from nitrogen analogues of carboxylic acids
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C255/00—Carboxylic acid nitriles
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Medicines Containing Antibodies Or Antigens For Use As Internal Diagnostic Agents (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
Conform inventiei, procedeul pentru prepararea acidului N-[3-(1*-3*-oxapentametilenamino-etilidenamino)-2,4,6-triiodbenzioil]-beta-amino-alfa-metilpropionic cu formula generala I: (vezi formula) consta în aceea ca, se trateaza (vezi formula) cu 1 pîna la 3 echivalenti molari, de preferinta 2 pîna la 3 echivalenti molari, N-acetilmorfolina si 1 pîna la 6 echivalenti molari, de preferinta 2 pîna la 6 echivalenti molari, oxiclorura de fosfor la o temperatura de 0 pîna 10 degree C, de preferinta 0...5 degree C, si se lasa reactantii sa reactioneze la temperaturi cuprinse între 10 degree C si punctul de fierbere al amestecului de reactie obtinut în apa în timpul sau dupa evaporarea solventului, se separa eventual partile insolubile existente de solutia acida rezultata si se precipita prin alcalinizare la un pH de cel putin 8, nitrilul cu formula II: (vezi formula) care se izoleaza si eventual se purifica, dupa care se trece acest nitril în acidul liber, prin metode în sine cunoscute.According to the invention, the process for the preparation of N- [3- (1'-3'-oxapentamethyleneamino-ethylideneamino) -2,4,6-triiodobenzoyl] -beta-amino-alpha-methylpropionic acid of general formula I in that 1 to 3 molar equivalents, preferably 2 to 3 molar equivalents, N-acetylmorpholine and 1 to 6 molar equivalents, preferably 2 to 6 molar equivalents, are treated (see formula) with phosphorous oxychloride at a temperature of 0 to 10 ° C, preferably 0-5 ° C, and let the reactants react at temperatures between 10 ° C and the boiling point of the reaction mixture obtained in the water during or after evaporation of the solvent , eventually separating the insoluble parts of the resulting acidic solution and precipitating by alkalinisation to a pH of at least 8, the nitrile of the formula II: (see formula) which is isolated and eventually purified, and then this nitrile is passed into the free acid , by methods known per se ute.
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE19803000215 DE3000215A1 (en) | 1980-01-04 | 1980-01-04 | Iomorinic acid prodn. useful as X=ray contrast agent - by reacting amino-tri:iodo:benzoyl-amino-methyl propionitrile with N-acetyl:morpholine followed by hydrolysis |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| RO81056B true RO81056B (en) | 1983-05-30 |
| RO81056A RO81056A (en) | 1983-06-01 |
Family
ID=6091548
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| RO80103041A RO81056A (en) | 1980-01-04 | 1980-12-30 | PROCESS FOR PREPARATION OF N- (3- (1 ', 3'-OXAPENTIAMETHENAMINOETILIDENAMINO) -2,4,6-TRIODOBENZOYL) -BETA-AMINO-ALFA-METHYLPROPIONIC ACID |
Country Status (10)
| Country | Link |
|---|---|
| CS (1) | CS216545B2 (en) |
| DD (1) | DD155901A1 (en) |
| DE (1) | DE3000215A1 (en) |
| ES (1) | ES8201148A1 (en) |
| HU (1) | HU180185B (en) |
| PL (1) | PL127295B1 (en) |
| PT (1) | PT72221B (en) |
| RO (1) | RO81056A (en) |
| SU (1) | SU980618A3 (en) |
| YU (1) | YU309780A (en) |
-
1980
- 1980-01-04 DE DE19803000215 patent/DE3000215A1/en not_active Withdrawn
- 1980-12-08 YU YU309780A patent/YU309780A/en unknown
- 1980-12-18 PT PT7222180A patent/PT72221B/en unknown
- 1980-12-26 SU SU803221254A patent/SU980618A3/en active
- 1980-12-28 HU HU312780A patent/HU180185B/en unknown
- 1980-12-30 DD DD22672780A patent/DD155901A1/en unknown
- 1980-12-30 ES ES498238A patent/ES8201148A1/en not_active Expired
- 1980-12-30 RO RO80103041A patent/RO81056A/en unknown
-
1981
- 1981-01-02 PL PL22904181A patent/PL127295B1/en unknown
- 1981-01-04 CS CS4981A patent/CS216545B2/en unknown
Also Published As
| Publication number | Publication date |
|---|---|
| CS216545B2 (en) | 1982-11-26 |
| DD155901A1 (en) | 1982-07-14 |
| ES498238A0 (en) | 1981-12-01 |
| ES8201148A1 (en) | 1981-12-01 |
| PL127295B1 (en) | 1983-10-31 |
| RO81056A (en) | 1983-06-01 |
| SU980618A3 (en) | 1982-12-07 |
| PT72221A (en) | 1981-01-01 |
| YU309780A (en) | 1983-01-21 |
| DE3000215A1 (en) | 1981-07-09 |
| PT72221B (en) | 1981-11-02 |
| HU180185B (en) | 1983-02-28 |
| PL229041A1 (en) | 1981-10-16 |
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