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Water → Lithium [4-(morpholin-4-yl)-6-oxo-1,6-dihydropyrimidin-2-yl]acetate

HRID 880056
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HRID 880056 반응식
O.[OH-].[Li+:3].[N:4]1([C:10]2[N:11]=[C:12]([CH2:17][C:18]([O:20]CC)=[O:19])[NH:13][C:14](=[O:16])[CH:15]=2)[CH2:9][CH2:8][O:7][CH2:6][CH2:5]1>CO>[N:4]1([C:10]2[N:11]=[C:12]([CH2:17][C:18]([O-:20])=[O:19])[NH:13][C:14](=[O:16])[CH:15]=2)[CH2:5][CH2:6][O:7][CH2:8][CH2:9]1.[Li+:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 3939Lithium HydroxideHCID 135905419Ethyl 2-[4-(morpholin-4-yl)-6-oxo-1,6-dihydropyrimidin-2-yl]acetate

생성물 1

HCID 136041845Lithium [4-(morpholin-4-yl)-6-oxo-1,6-dihydropyrimidin-2-yl]acetate수율 94.3%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

7.5 ml of water and 197 mg of lithium hydroxide are added to a solution of 2 g of ethyl [4-(morpholin-4-yl)-6-oxo-1,6-dihydropyrimidin-2-yl]acetate prepared in stage 1 of Example 1 in 75 ml of methanol. After stirring for 48 hours at ambient temperature, the reaction mixture is concentrated under reduced pressure. 50 ml of water are added. The aqueous phase is then washed with ethyl acetate and then lyophilized. 1.73 g of lithium [4-(morpholin-4-yl)-6-oxo-1,6-dihydropyrimidin-2-yl]acetate are obtained in the form of a white solid, the characteristics of which are similar to the product of stage 2.

후처리

  1. concentrationthe reaction mixture is concentrated under reduced pressure
  2. addition50 ml of water are added
  3. washThe aqueous phase is then washed with ethyl acetate

출처 및 근거

ORD 기록
ord-5e2f1c81ec3040dcb4da78298de02a36
출처 데이터셋
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08993565B2

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