Alternatived Products of [ 71463-50-8 ]
Product Details of [ 71463-50-8 ]
CAS No. : | 71463-50-8 |
MDL No. : | MFCD00033180 |
Formula : |
C9H5Cl2NO
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Boiling Point : |
- |
Linear Structure Formula : | - |
InChI Key : | - |
M.W : |
214.05
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Pubchem ID : | - |
Synonyms : |
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Safety of [ 71463-50-8 ]
Signal Word: | |
Class: | |
Precautionary Statements: | |
UN#: | |
Hazard Statements: | |
Packing Group: | |
Application In Synthesis of [ 71463-50-8 ]
* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
- Downstream synthetic route of [ 71463-50-8 ]
- 1
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[ 151-50-8 ]
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[ 81547-72-0 ]
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[ 71463-50-8 ]
- 2
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[ 2040-05-3 ]
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[ 71463-50-8 ]
- 3
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[ 14920-87-7 ]
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[ 75-05-8 ]
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[ 71463-50-8 ]
Yield | Reaction Conditions | Operation in experiment |
67% |
With lithium diisopropyl amide In tetrahydrofuran at -78 - 20℃; for 2h; Inert atmosphere; |
|
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Stage #1: acetonitrile With n-butyllithium In tetrahydrofuran; hexane at -78℃; for 0.75h;
Stage #2: 2,6-dichlorobenzoic acid methyl ester In tetrahydrofuran; hexane at -78℃; for 0.5h;
Stage #3: With methanol In tetrahydrofuran; hexane |
151
n-Butyl lithium (20.1 mL, 32.2 mmol, 1.6M in hexanes) was added to THF (30 mL) and the solution was cooled to - 78 °C. Acetonitrile (1.7 mL, 32 mmol) was added dropwise and the reaction stirred at the temperature for 45 minutes. Methyl 2,6-dichlorobenzoate (1.00g, 4.88 mmol) was dissolved in 2 mL THF and added to the reaction mixture. The reaction stirred at -78 °C for 0.5 hr. The solution was quenched with methanol and warmed to room temperature. The material was diluted with water and 1N HC1. The solution was then extracted with Ethyl acetate, dried, and concentrated to give 1.08g of desired product at 85% purity. Material used as is in the next step. @H-NMR (CDC13) No.: 4. 0 (s, 2H) , 7.28 - 7. 40 (m, 3H) . |
Reference:
[1]Vogl, Michael; Brecker, Lothar; Kratzer, Regina; Nidetzky, Bernd
[Chirality, 2012, vol. 24, # 10, p. 847 - 853,7]
[2]Current Patent Assignee: TAKEDA PHARMACEUTICAL COMPANY LIMITED - WO2005/99688, 2005, A2
Location in patent: Page/Page column 305-306