Phthaloyl amlodipine synthesis
- Product Name:Phthaloyl amlodipine
- CAS Number:88150-62-3
- Molecular formula:C28H27ClN2O7
- Molecular Weight:538.98
89-98-5
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14205-39-1
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![ETHYL4-[2-(1,3-DIOXO-1,3-DIHYDRO-2H-ISOINDOL-2-YL)ETHOXYL]-3-OXOBUTANOATE](/CAS/GIF/88150-75-8.gif)
88150-75-8
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$85.00/100mg
88150-62-3
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$49.00/25mg
Yield:88150-62-3 76.1%
Reaction Conditions:
Stage #1:2-chloro-benzaldehyde;ethyl 4-[2-(phthalimido)ethoxy]acetoacetate with piperidine;acetic acid in isopropyl alcohol;toluene at 20 - 30;Large scale;
Stage #2:methyl (E)-3-aminocrotonate in isopropyl alcohol;toluene at 55 - 58; for 7 h;Large scale;
Steps:
3 (3) Synthesis of phthaloyl amlodipine
To a solution of ethyl 4-(2-phthalimidoethoxy)acetoacetate in toluene was added 3000 ml of isopropyl alcohol, 564 g of 2-chlorobenzaldehyde was added with stirring, 17 5g acetic acid, 24.8g piperidine; 20 ~ 30 °C, stirring 9 ~ 10h, adding 589g β-aminocrotonic acid methyl ester, heating to 55 ~ 58 °C, and stirring at 55 ~ 58 °C reaction, stirring 7h sampling, TLC plate to confirm the end of the reaction, cooling to below 25 °C, adding 3200ml acetic acid; then seeded to 0 ~ 5 °C, the same temperature for 5h, crystallization; filtration crystallization, with 800ml isopropyl alcohol washing, the wash was run twice (400 ml each) and dried under reduced pressure to give 1611 g of phthaloyl amlodipine in a yield of 76.1%.
References:
Qianhui Pharmaceutical (Anhui) Co., Ltd.;Yang Huilai;Mao Jie;Sun Xuexi CN106749187, 2017, A Location in patent:Paragraph 0035; 0036; 0037
89-98-5
635 suppliers
$18.00/25g
88150-75-8
137 suppliers
$85.00/100mg
14205-39-1
496 suppliers
$6.00/25g
88150-62-3
257 suppliers
$49.00/25mg
![2-[(2-Chlorophenyl)Methylene]-4-[2-(1,3-dihydro-1,3-dioxo-2H-isoindol-2-yl)ethoxy]-3-oxobutanoic Acid Ethyl Ester](/CAS/20150408/GIF/400024-08-0.gif)
400024-08-0
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14205-39-1
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88150-62-3
257 suppliers
$49.00/25mg
89-98-5
635 suppliers
$18.00/25g
21731-17-9
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88150-75-8
137 suppliers
$85.00/100mg
88150-62-3
257 suppliers
$49.00/25mg
3891-07-4
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88150-62-3
257 suppliers
$49.00/25mg