3-ChloroMethyl-pyridine 1-oxide synthesis
- Product Name:3-ChloroMethyl-pyridine 1-oxide
- CAS Number:82401-08-9
- Molecular formula:C6H6ClNO
- Molecular Weight:143.57
6959-48-4
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Yield:82401-08-9 29%
Reaction Conditions:
Stage #1: 3-chloromethylpyridinium chloridewith sodium hydrogencarbonate in water at 0;
Stage #2: with peracetic acid;acetic acid in chloroform; for 18 h;
Steps:
1 EXAMPLE 1
Picolyl chloride hydrochloride (8.0 g, 49 mmol) is dissolved in ice cold, saturated, aqueous sodium bicarbonate (100 ML) and the mixture is extracted with 2 X 100 mL chloroform. The chloroform extracts are dried (MGS04) and filtered. 32% Peracetic acid in acetic acid (50 mL) is added to the filtrate and the mixture is vigorously stirred for 18 h. The mixture is washed twice with cold, sat. , aq. NAHCO3, dried (MGS04), and concentrated in vacuo. The solid obtained is triturated with hexanes and dried in vacuo to give 3-chloromethylpyridine N-oxide (2.0 g, 29% yield) as a white crystalline solid.
References:
WO2004/46113,2004,A2 Location in patent:Page 51-52
6968-72-5
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3099-31-8
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100-55-0
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