반응 #68085

반응 방정식

sodium hydroxide

ethyl 1-(2-(2,3-dihydro-1,4-benzodioxin-6-yl)ethyl)-4-(2-(7-methoxy-4-methyl-2-oxoquinolin-1(2H)-yl)ethyl)piperazine-2-carboxylate

sodium hydroxide

→

1-(2-(2,3-dihydro-1,4-benzodioxin-6-yl)ethyl)-4-(2-(7-methoxy-4-methyl-2-oxoquinolin-1(2H)-yl)ethyl)piperazine-2-carboxylic acid

수율 63.7%

용매

methanol

methanol

반응 조건

후처리

1. 1
   workup.ADDITIONwas added
2. 2
   workup.STIRRINGstirred at room temperature for 6 hours
3. 3
   기타After the solvent was removed under reduced pressure, water
4. 4
   workup.ADDITIONwas added
5. 5
   workup.ADDITIONethanol was added
6. 6
   여과The resulting solid was filtered

실험 절차

To 3.3 mL of a 90% aqueous methanol solution containing 58 mg of ethyl 1-(2-(2,3-dihydro-1,4-benzodioxin-6-yl)ethyl)-4-(2-(7-methoxy-4-methyl-2-oxoquinolin-1(2H)-yl)ethyl)piperazine-2-carboxylate, 22 mg of sodium hydroxide was added and stirred at room temperature for 30 min. Further, 66 mg of sodium hydroxide and 1.1 mL of a 90% aqueous methanol solution were added and stirred at room temperature for 6 hours. After the solvent was removed under reduced pressure, water was added, and adjusted to pH 1 with 6.0 mol/L hydrochloric acid, thereafter ethanol was added and adjusted to pH 6.5 with aqueous saturated sodium hydrogen carbonate solution and 1.0 mol/L hydrochloric acid. The resulting solid was filtered to give 35 mg of 1-(2-(2,3-dihydro-1,4-benzodioxin-6-yl)ethyl)-4-(2-(7-methoxy-4-methyl-2-oxoquinolin-1(2H)-yl)ethyl)piperazine-2-carboxylic acid as a white solid.

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