N-(1,3-benzodioxol-5-ylmethyl)-2,2-dimethylpropanamide synthesis
- Product Name:N-(1,3-benzodioxol-5-ylmethyl)-2,2-dimethylpropanamide
- CAS Number:120226-50-8
- Molecular formula:C13H17NO3
- Molecular Weight:235.28
2620-50-0
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Yield:120226-50-8 92.6%
Reaction Conditions:
with triethylamine in dichloromethane at 0 - 20; for 2.16667 h;
Steps:
1 Synthesis of 7,8-dihydro-6H_ [1,3] dioxolo [4,5_e] isoindole hydrochloride
400 g of compound 7,400 g of triethylamine and 2000 g of dichloromethane were added to a 3000 mL three-necked flask, stirred for 10 min,Ice bath cooling to 0 -5 ; start slowly dropping 380g pivaloyl chloride, control the internal temperature is less than 10 , after the drop is completed,The reaction was stirred at room temperature, controlled by TLC, reacted for 2 hours. After the reaction, the pH was adjusted to 6-7 with 1N 0.5N dilute hydrochloric acid,Phase with water (1000mL) wash twice, 150g yuan Ming powder drying, pumping filter, under reduced pressure, petroleum ether beating, pumping, vacuum dryingTo 576 g of compound 6 in a yield of 92.6%,
References:
CN106366089,2017,A Location in patent:Paragraph 0072; 0073; 0074