3,4-DIFLUOROBENZOIC ACID HYDRAZIDE synthesis
- Product Name:3,4-DIFLUOROBENZOIC ACID HYDRAZIDE
- CAS Number:229957-07-7
- Molecular formula:C7H6F2N2O
- Molecular Weight:172.13
369-25-5
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Yield:229957-07-7 100%
Reaction Conditions:
with hydrazine hydrate in methanol at 20; for 1.5 h;Inert atmosphere;
Steps:
5 Synthesis of Intermediate 54
Under the protection of nitrogen, 2.0 g (11.62 mmol) of material 53 was dissolved in 20 ml of methanol, added with 8.2 ml (139.44 mmol, 85%) of hydrazine hydrate, and reacted at room temperature for 1.5 h. The reaction was monitored by TLC (PE/EA=3:1). After the reaction was completed, the resulting mixture was added with 50 ml of water and stirred to precipitate out a solid, filtered, washed with water, and pumped to dryness. The aqueous phase was extracted with EA. The organic phase was dried, concentrated by rotary evaporation, and pumped to dryness to give a product (2 g), as a white solid. Yield: 100%. LC-MS: 173 [M+1]+, tR=2.528 min.
References:
US2021/347745,2021,A1 Location in patent:Paragraph 0199-0200
76903-88-3
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455-86-7
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