반응 #437793

반응 방정식

product

N-(2-formyl-4-methoxyphenyl)formamide

L-glutamine

sodium borohydride

→

4-carbamoyl-2-(6-methoxy-4H-quinazolin-3-yl)butanoic acid

용매

sodium hydroxide

methanol

methanol

sodium hydroxide

반응 조건

후처리

1. 1
   온도the mixture was cooled to 0° C.
2. 2
   workup.STIRRINGThe mixture was stirred for 12 hours at 0° C.
3. 3
   workup.STIRRINGstirred for a further 4 hours at 20° C
4. 4
   workup.DISTILLATIONthe methanol was distilled off
5. 5
   세척The aqueous residue was washed twice with 15 ml of diethyl ether each time
6. 6
   농축concentrated by evaporation in vacuo
7. 7
   여과freed from insoluble constituents by filtration
8. 8
   기타The residue obtained
9. 9
   기타by evaporating the filtrate in vacuo
10. 10
    기타as described in stage 5, without purification

실험 절차

A solution of 0.79 g of the product from stage 3 in 30 ml of methanol was added to a solution of 0.58 g of L-glutamine in 10 ml of methanol and 2 ml of 2N sodium hydroxide solution. After stirring for 1 hour at 20° C., the mixture was cooled to 0° C. and 0.103 g of sodium borohydride was added in portions within 30 minutes. The mixture was stirred for 12 hours at 0° C., then adjusted to pH 2 to 3, and stirred for a further 4 hours at 20° C. After neutralizing the solution with sodium hydroxide, the methanol was distilled off. The aqueous residue was washed twice with 15 ml of diethyl ether each time, and then concentrated by evaporation in vacuo. The residue was taken up in 25 ml of methanol and freed from insoluble constituents by filtration. The residue obtained by evaporating the filtrate in vacuo was directly reacted further as described in stage 5, without purification.

출처