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2-Amino-2,3-dimethylbutanamide → HCID 178439576, 화합물

HRID 358848
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HRID 358848 반응식
[CH3:1][O-].[Na+].C([O:6][C:7]([C:9]1[C:14](C(OCC)=O)=[CH:13][CH:12]=[C:11]([CH:20]2[CH2:22][CH2:21]2)[N:10]=1)=[O:8])C.[NH2:23][C:24]([CH3:31])([CH:28]([CH3:30])[CH3:29])[C:25]([NH2:27])=[O:26]>CO.C(O)C>[CH:20]1([C:11]2[NH:10][C:9]([C:1]3[NH:23][C:24]([CH:28]([CH3:30])[CH3:29])([CH3:31])[C:25](=[O:26])[N:27]=3)([C:7]([OH:6])=[O:8])[CH:14]=[CH:13][CH:12]=2)[CH2:21][CH2:22]1
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참가 물질

6

반응물 3

HCID 97937732-Amino-2,3-dimethylbutanamideHCID 10942334Sodium MethoxideHCID 142803436-Cyclopropylpyridine-2,3-dicarboxylic acid diethyl ester

생성물 1

HCID 178439576HCID 178439576, 화합물수율 57.9%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 887Methanol
용매

실험 절차

10 g of 30% sodium methoxide in methanol are added to a solution of 6 g of 6-cyclopropylpyridine-2,3-dicarboxylic acid diethyl ester and 3 g of 2-amino-2,3-dimethylbutyramide in 100 ml of ethanol and the reaction mixture is boiled under reflux for 3 hours. It is then concentrated, the residue is dissolved in a small amount of water, and the solution is saturated with sodium chloride. The pH is then adjusted to 4 with concentrated hydrochloric acid and the solution is extracted three times with 150 ml of ethyl acetate each time. The organic phase is dried over magnesium sulphate, filtered and concentrated. The residue crystallises from ether/hexane 1:2. In this manner 4 g of 6-cyclopropyl-2-(5-isopropyl-5-methyl-4-oxoimidazolin-2-yl)-pyridinecarboxylic acid having a melting point of 118°-121° are obtained.

후처리

  1. temperatureunder reflux for 3 hours
  2. concentrationIt is then concentrated
  3. dissolutionthe residue is dissolved in a small amount of water
  4. extractionthe solution is extracted three times with 150 ml of ethyl acetate each time
  5. dry with materialThe organic phase is dried over magnesium sulphate
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customThe residue crystallises from ether/hexane 1:2

출처 및 근거

ORD 기록
ord-46dcbf34d7e349ff9246061a2d2f5548
출처 데이터셋
uspto-grants-1991_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04997947

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