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ChemicalBook CAS DataBase List N-Methoxy-N-Methyl 5-broMo-2-chlorobenzaMide
842136-59-8

N-Methoxy-N-Methyl 5-broMo-2-chlorobenzaMide synthesis

4synthesis methods
-

Yield:842136-59-8 99%

Reaction Conditions:

Stage #1: N,O-dimethylhydroxylamine*hydrochloridewith triethylamine in dichloromethane at -10 - 10; for 0.5 h;
Stage #2: 5-bromo-2-chloro-benzoyl chloride in dichloromethane; for 3 h;

Steps:

2 Example 2 Preparation of Compound B

To 250mL single-neck flask methoxymethyl amine hydrochloride (9.75g, 100mmol, 2.5eq) and dichloromethane (90mL), stirred and the reaction temperature is -10 ~ 10°C,Slowly add 22 mL of triethylamine, 160 mmol, 4.0 eq), and stir for 30 minutes.A solution of the above compound A (10.20 g, 40 mmol, 1.0 eq) dissolved in dichloromethane (15 mL) was slowly added dropwise.After the addition is complete, continue stirring for 3 hours. After returning to room temperature, the reaction solution was washed with 100 mL of water, and the organic phase was washed with 100 saturated sodium chloride and separated.The organic phase was dried over anhydrous Na 2 SO.Vacuum drying to give a white solid 11.0 g. The yield was 99%, which is the compound B.

References:

CN108314613,2018,A Location in patent:Paragraph 0012; 0034; 0035

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