2-ACETOXY-3-METHOXYBENZALDEHYDE 97 synthesis
- Product Name:2-ACETOXY-3-METHOXYBENZALDEHYDE 97
- CAS Number:7150-01-8
- Molecular formula:C10H10O4
- Molecular Weight:194.18
Yield:7150-01-8 98%
Reaction Conditions:
with dmap;triethylamine in dichloromethane at -20 - 20; for 12 h;
Steps:
1.1 Synthesis of 2-acetoxy-3-methoxy-benzaldehyde
2-hydroxy-3-methoxy-benzaldehyde (30.4 g, 200 mmol)Add to dichloromethane (20 mL),After the 2-hydroxy-3-substituted-benzaldehyde is dissolved,4-Dimethylaminopyridine (0.24 g, 2 mmol) was added in sequence.Triethylamine (27.9 mL, 200 mmol).At -20 ° C,Acetyl chloride (15.7 g, 200 mmol) was slowly added dropwise using a constant pressure dropping funnel.The temperature was maintained at 0 ° C during the dropwise addition.After the addition is completed,Slowly raise the reaction temperature to room temperature.And reacted at room temperature for 12 h.The reaction solution was poured into 2N hydrochloric acid (350 mL).Separating the organic phase,The aqueous phase was extracted with dichloromethane (200 mL×3).Combine the organic phase,Dry with anhydrous sodium sulfate, suction filtration,Rotating to remove the solvent,The product was recrystallized from ethanol.A yellow solid (38.1 g, yield 98%) was obtained.
References:
CN108358761,2018,A Location in patent:Paragraph 0038; 0039
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