4-(2-METHOXY-5-METHYL-PHENYL)-4-OXO-BUTYRIC ACID synthesis
- Product Name:4-(2-METHOXY-5-METHYL-PHENYL)-4-OXO-BUTYRIC ACID
- CAS Number:55007-22-2
- Molecular formula:C12H14O4
- Molecular Weight:222.24
108-30-5
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104-93-8
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55007-22-2
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Yield:55007-22-2 1.6 kg
Reaction Conditions:
with aluminum (III) chloride in dichloromethane at -5 - 10;Large scale;
Steps:
1
1220 g (10 mOl, leq) of p-methylanisole (2) was added to 12 L of dichloromethane (room temperature)Cooling -5 ~ 0 degrees 1600g (12mol, 1. 2eq) of aluminum trichloride,After the addition 1200g of succinic anhydride (12mol, 1. 2eq) was added dropwise to the reaction system,After the temperature drops about 10 degrees reaction overnight.After completion of the reaction, 10 L of water was added dropwise and quenched, the layers were separated and the aqueous phase was extracted three times with dichloromethane (5 L * 3). The combined dichloromethane phases were washed with 5% sodium bicarbonate solution and saturated brine to neutral (5 L), dried over anhydrous sodium sulfate and dried over dichloromethane to give 1.6 kg of crude product (3) which was used in the next reaction without further purification.
References:
CN107382698,2017,A Location in patent:Paragraph 0048-0051
108124-66-9
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55007-22-2
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77-78-1
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55007-22-2
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