3-PYRIDAZINEMETHANOL, 6-CHLORO- synthesis
- Product Name:3-PYRIDAZINEMETHANOL, 6-CHLORO-
- CAS Number:1011487-94-7
- Molecular formula:C5H5ClN2O
- Molecular Weight:144.56
65202-50-8
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$21.21/1gm:
1011487-94-7
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Yield:-
Reaction Conditions:
Stage #1:methyl 6-chloro-3-pyridazinecarboxylate with diisobutylaluminium hydride in tetrahydrofuran at 0; for 0.333333 h;
Stage #2: with hydrogenchloride in tetrahydrofuran;water at 0;
Stage #3: with sodium hydrogencarbonate in tetrahydrofuran;water at 20;
Steps:
87.1
Example 87 [0264] Formula 88] [0265] 1) In tetrahydrofuran (100 mL) was dissolved methyl 6-chloropyridazin-3-carboxylate (1.726 g), the solution was cooled to 0°C, 1M diisobutyaluminum hydride-tetrahydro- furan solution (20 mL) was added dropwise to the solution, and the mixture was stirred at the same temperature for 20 minutes. To the reaction mixture were successively added water (10 mL) and IN hydrochloric acid (20 mL) at 0°C. After adding a saturated aqueous sodium bicarbonate solution to the mixture at room temperature, the mixture was extracted with chloroform. The extract was dried over anhydrous sodium sulfate, and the residue obtained by concentrating the extract under reduced pressure was purified by silica gel column chromatography (n-hexane: ethyl acetate=90: 10 to 25:75) to obtain (6-chloropyridazin-3-yl)methanol (177 mg).MS (m/z): 147/145 [M+H]+
References:
MITSUBISHI TANABE PHARMA CORPORATION;SAKURAI, Osamu;SARUTA, Kunio;HAYASHI, Norimitsu;GOI, Takashi;MOROKUMA, Kenji;TSUJISHIMA, Hidekazu;SAWAMOTO, Hiroaki;SHITAMA, Hiroaki;IMASHIRO, Ritsuo WO2012/81736, 2012, A1 Location in patent:Page/Page column 82
6531-04-0
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$279.23/1gm:
1011487-94-7
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$60.00/5mg
303085-53-2
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$75.00/100mg
1011487-94-7
47 suppliers
$60.00/5mg