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2-Amino-2,3-dimethylbutanamide → HCID 178439576、化合物

HRID 358848
ノート
印刷プレビュー

反応式

HRID 358848 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

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

生成物 1

HCID 178439576HCID 178439576、化合物収率 57.9%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 887Methanol
溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-46dcbf34d7e349ff9246061a2d2f5548
出典データセット
uspto-grants-1991_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04997947

反応ノート

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