4-Amino-5-chloro-2,3-dihydro-7-benzofurancarboxylic acid synthesis
- Product Name:4-Amino-5-chloro-2,3-dihydro-7-benzofurancarboxylic acid
- CAS Number:123654-26-2
- Molecular formula:C9H8ClNO3
- Molecular Weight:213.62
143878-29-9
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123654-26-2
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Yield:123654-26-2 89.8%
Reaction Conditions:
with 1-methoxy-2-propanol;water;sodium hydroxide at 90; for 8 h;
Steps:
7 Example 7 Synthesis of 4-amino-5-chloro-2,3-dihydrobenzofuran-7-carboxylic acid
The resulting intermediate 7 (30 g, 0.11 mol), water (150 mL),Propylene glycol monomethyl ether (36mL) and 50% sodium hydroxide solution (90mL), slowly heated to 90 ° C with stirring, the same temperature for 8h, the reaction was monitored by TLC. After the reaction is completed,Cooled to 5 ° C with ice bath and stirred for 2h, filtered with suction,The filter cake was washed with an appropriate amount of water added to 500mL single-necked flask,Water (210 mL) and propylene glycol monomethyl ether (35 mL) were added,The temperature of the reaction solution was raised to 80 ° C and the reaction solution became homogeneous.Dilute dilute hydrochloric acid, adjust pH to about 3, precipitated solid.After cooling to 10 ° C, stirring was continued for 2h. Suction filtration,The filter cake was washed with an appropriate amount of water and dried to give an off-white solid,Yield 20.8g, yield 89.8%, purity 99%
References:
CN107337658,2017,A Location in patent:Paragraph 0051; 0052
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