3-CHLORO-N-HYDROXY-2,2-DIMETHYL-PROPANAMIDE synthesis

Yield: 95.3%

Reaction Conditions:

with hydroxylamine hydrochloride;sodium hydroxide in water; pH=7.2 at -5 - 20; for 4.5 h;Concentration;Reagent/catalyst;

Steps:

1.1 Example 1
Step one In a 250 ml four-necked flask was added 18.8 g (0.26 mol)Hydroxylamine hydrochloride and 100 ml of distilled water, 2 g of ether catalyst,In the ice salt bath (-5 ~ 0 ) stirring,A solution of 30% NaOH was added dropwise so that the pH of the solution reached 7.2.Then dripChloride pivalyl chloride 6ml (0.2mol), while dropping 30% NaOH solution, the system to maintain pH7.2 ± 0.1.1.5hInside the drop finished, room temperature stirring3h. After completion of the reaction, it was filtered and dried to give a white solid which was 3-chloro-N-hydroxy-2,2-dimethylpropanamide. content99.0% (HPLC) yield 95.3%.

References:

Jiangsu Changqing Biological Technology Co., Ltd.;Yu Guoquan;Sun Xialin;Ding Huaping;Zhou Peng;Yuan Yu;Lv Jiahang CN106749072, 2017, A Location in patent:Paragraph 0016; 0019; 0022; 0025