Alternatived Products of [ 1111638-41-5 ]
Product Details of [ 1111638-41-5 ]
CAS No. : | 1111638-41-5 |
MDL No. : | N/A |
Formula : |
C7H7BrClNO
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Boiling Point : |
- |
Linear Structure Formula : | - |
InChI Key : | - |
M.W : |
236.49
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Pubchem ID : | - |
Synonyms : |
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Safety of [ 1111638-41-5 ]
Application In Synthesis of [ 1111638-41-5 ]
* 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.
- Upstream synthesis route of [ 1111638-41-5 ]
- Downstream synthetic route of [ 1111638-41-5 ]
- 1
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[ 75-16-1 ]
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[ 228251-24-9 ]
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[ 1111638-41-5 ]
Yield | Reaction Conditions | Operation in experiment |
73.6% |
|
Preparation of 1-(5-bromo-2-chloropyridin-3-yl)ethanol (D-2-4).To a stirred solution of compound D-2-3 (8.0 g, 36.3 mmol) in dry THF (100 mL) was added a solution of 3 M CH3MgBr in THF (18.14 mL, 54.4 mmol) dropwise at -78 0C under N2 atmosphere. After the addition, the resulting mixture was allowed to warmed up to room temperature and stirred overnight. TLC (petroleum ether/EtOAc 8:1 ) indicated most of compound D-2-3 was consumed. H2O (200 mL) was added to the reaction mixture and the mixture was extracted with EtOAc (100 mL*3). The combined organic layers were washed with saturated aqueous NaCI (200 mL), dried over Na2SO4 and concentrated in vacuo to give crude compound D-2-4, which was purified by column chromatography (silica gel, petroleum ether/EtOAc 50:1 ) to yield pure compound D-2-4 (6.3 g, 73.6%) as a yellow oil. |
- 2
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[ 1111638-41-5 ]
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[ 886365-47-5 ]
Yield | Reaction Conditions | Operation in experiment |
77% |
With pyridine; chromium(VI) oxide; In dichloromethane; at 0 - 20℃;Silica gel; |
Preparation of 1-(5-bromo-2-chloropyridin-3-yl)ethanone (D-2-5). <n="106"/>To a stirred solution of pyridine (13 g, 0.165 mol) in CH2CI2 (200 mL) was added CrO3 (8.25 g, 0.083 mol) and silica gel (20 mL) portionwise at 0 C. After the addition, the reaction mixture was stirred for 10 minutes. Compound D-2-4 (6.5 g, 27.5 mmol) was then added and the resulting mixture was stirred at room temperature overnight. TLC (petroleum ether/EtOAc 8:1 ) indicated most of compound D-2-4 was consumed. The reaction mixture was filtered and the filtrate was concentrated in vacuo to give crude compound D-2-5, which was purified by column chromatography (silica gel petroleum ether/EtOAc 20:1) to give pure compound D-2-5 (5 g, yield: 77%) as a yellow oil. |