3-(1,3-benzodioxol-5-yl)-3-oxopropanenitrile synthesis
- Product Name:3-(1,3-benzodioxol-5-yl)-3-oxopropanenitrile
- CAS Number:96220-14-3
- Molecular formula:C10H7NO3
- Molecular Weight:189.17
Yield:96220-14-3 91%
Reaction Conditions:
with sodium hydride in tetrahydrofuran at 70; for 5.5 h;Cooling with ice;
Steps:
1 N- (3- (benzo [d] [1,3] dioxol-5-yl) -1H-pyrazol-5-yl) -4-((1-methylpiperidine-4 -Yl) amino) benzamide (1)
Add tetrahydrofuran (12ml), acetonitrile (5mL), sodium hydride (0.17g, 7.1mmol), and benzo [d] [1,3] dioxolene-5 to the round-bottomed flask in this order in an ice bath. -Methyl formate (0.43 g, 2.4 mmol), stirred for 0.5 h, then warmed to reflux and reacted for 5 h.The reaction solution was poured into an ice-water mixture (30 ml), the pH was adjusted to 2, and a large amount of a yellow solid precipitated, which was filtered with suction and dried to obtain a crude product.The crude product was subjected to column chromatography (PE: EA = 2: 1) to obtain 0.413 g of a pale yellow solid with a yield of 91%.
References:
CN110835336,2020,A Location in patent:Paragraph 0146-0149; 0177-0179
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