(4-(hydroxyimino)methyl)-2-methylbenzoic acid synthesis
- Product Name:(4-(hydroxyimino)methyl)-2-methylbenzoic acid
- CAS Number:1437051-93-8
- Molecular formula:C9H9NO3
- Molecular Weight:179.17
503470-23-3
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Yield:1437051-93-8 91.2%
Reaction Conditions:
with hydroxylamine hydrochloride;sodium acetate in tetrahydrofuran;water at 50; for 6 h;
Steps:
1.1.1; 1.1.2; 1.1.3 Hydroxylamine oximation
1) In a 500 ml round bottom flask, 150 ml of THF, 100 ml of water and 34.5 g (0.21 mol) of the intermediate 0 were successively added. After the solution was stirred and dissolved, 16.7 g (0.24 mol) of hydroxylamine hydrochloride was added, followed by the addition of 26.2 g of sodium acetate ( 0.32 mol). The reaction solution was stirred at 50 ° C for 6 hours;2) The reaction was stopped: 300 ml of water was successively added to the reaction liquid, and ethyl acetate 150 ml × 3 times to extract an aqueous phase. After combining the ethyl acetate phases, the organic phase is dried over anhydrous sodium sulfate;3) Ethyl acetate was evaporated under reduced pressure at 45 to 50 ° C to give Intermediate 1 34.3 g, yield 91.2%.Intermediate 1 can be directly fed to the subsequent reaction without further treatment.
References:
CN109879826,2019,A Location in patent:Paragraph 0075; 0076; 0077; 0078; 0079; 0080; 0081-0083
68837-59-2
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78775-11-8
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