2,2-dichloro-N,N-dimethylacetamide synthesis
- Product Name:2,2-dichloro-N,N-dimethylacetamide
- CAS Number:5468-76-8
- Molecular formula:C4H7Cl2NO
- Molecular Weight:156.01
Yield:5468-76-8 92.1%
Reaction Conditions:
with sodium hydroxide in dichloromethane at 0 - 5;Temperature;
Steps:
1-8; 12.1 Preparation of Intermediate 1
200ml of methylene chloride was put into the reaction flask, and dimethylamine gas was introduced, so that the molar amount of dimethylamine reagent introduced was 2 times that of dichloroacetyl chloride, (the dimethylamine gas was composed of a 40% dimethylamine solution. Add sodium hydroxide to prepare), control the reaction temperature to 0 ~ 5 , and dropwise add a dichloromethane solution (1 g/ml) containing 50.0 g of dichloroacetyl chloride. After the reaction was completed, the pH was adjusted to 7-8 by adding acid. Stir and let stand for 20-30 minutes, separate the layers and collect the organic layer. Drying under reduced pressure gave 47.85 g of intermediate 1 (N,N-dimethyl-2,2-dichloroacetamide). After testing, the yield was 92.1% and the purity was 99.66%.
References:
CN114057725,2022,A Location in patent:Paragraph 0067-0091; 0111-0116
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