ChemicalBook CAS DataBase List N-(3,4-DIMETHOXYPHENETHYL)ACETAMIDE

N-(3,4-DIMETHOXYPHENETHYL)ACETAMIDE synthesis

12synthesis methods

Product Name:N-(3,4-DIMETHOXYPHENETHYL)ACETAMIDE
CAS Number:6275-29-2
Molecular formula:C12H17NO3
Molecular Weight:223.27

120-20-7
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75-36-5 Synthesis

75-36-5
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6275-29-2
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Yield:6275-29-2 100%

Reaction Conditions:

with triethylamine in dichloromethane at 0 - 26;Temperature;

Steps:

1.1

The specific operation is as follows: Mechanical stirring is installed on a 1L three-neck round bottom flask. Constant pressure dropping funnel and built-in thermometer; outside is ethanol circulating coolant.90.56 g (0.5 mol) of 3,4-dimethoxyphenethylamine, 100 mL (0.72 mol) of triethylamine and 455 mL of dichloromethane were successively added to the reaction flask. With stirring, the above mixture was reduced to 0°C. Then, 0.60 mol of acetyl chloride or acetic anhydride was weighed and transferred to a constant pressure dropping funnel; acetyl chloride or acetic anhydride was added dropwise to the above reaction solution at an internal temperature of 0°C; the dropping time lasted for about 20-30 minutes. After completion of the addition, the reaction was carried out at 0°C for 30-60 minutes; then, the temperature was gradually raised to room temperature (25-26°C) and stirring was continued for 30 minutes. TLC showed the reaction was complete. The post-treatment of the reaction was: the reaction was transferred to a 1 L separatory funnel, washed with water (200 mL x 1), 3% Wash with dilute aqueous hydrochloric acid (200mL x 1), wash with saturated aqueous sodium bicarbonate solution (200mL x 1) and saturated brine (200mLx1). The organic phase was dried over anhydrous magnesium sulfate and filtered to give a filtrate. The filtrate was concentrated under reduced pressure on a rotary evaporator to give a white solid product, 112 g, compound number: SM-1-a, N-acetyl-3,4-dimethoxyphenylethylamine, 100% yield; English name: N-(3,4-dimethoxyphenethyl)acetamide.

References:

CN107540596,2018,A Location in patent:Paragraph 0050-0053; 0073