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Sodium Acetate → tert-butyl 4-[4-amino-5-(ethoxycarbonyl)-1H-pyrrol-3-yl]piperidine-1-carboxylate

HRID 1616086
ノート
印刷プレビュー

反応式

HRID 1616086 の反応式
[C:1]([CH:3]([CH:6]1[CH2:11][CH2:10][N:9]([C:12]([O:14][C:15]([CH3:18])([CH3:17])[CH3:16])=[O:13])[CH2:8][CH2:7]1)[CH:4]=O)#[N:2].Cl.[NH2:20][CH:21](C(OCC)=O)[C:22]([O:24][CH2:25][CH3:26])=[O:23].C([O-])(=O)C.[Na+].[O-]CC.[Na+]>CO.O>[NH2:2][C:1]1[C:3]([CH:6]2[CH2:11][CH2:10][N:9]([C:12]([O:14][C:15]([CH3:18])([CH3:17])[CH3:16])=[O:13])[CH2:8][CH2:7]2)=[CH:4][NH:20][C:21]=1[C:22]([O:24][CH2:25][CH3:26])=[O:23]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 517045Sodium AcetateHCID 2723922Sodium ethoxideHCID 3084143Propanedioic acid, 2-amino-, 1,3-diethyl ester, hydrochloride (1:1)HCID 86681870Tert-butyl 4-(1-cyano-2-oxoethyl)piperidine-1-carboxylate

生成物 1

HCID 86681878tert-butyl 4-[4-amino-5-(ethoxycarbonyl)-1H-pyrrol-3-yl]piperidine-1-carboxylate収率 46%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

The tert-butyl 4-(1-cyano-2-oxoethyl)piperidine-1-carboxylate (757 mg, 3.0 mmol) obtained in Step 4 of Example 1 was dissolved in methanol (6 mL) and water (2 mL), diethyl aminomalonate hydrochloride (952 mg, 4.5 mmol) and sodium acetate (492 mg, 6.0 mmol) were added, followed by stirring at room temperature for 18 hours. The reaction liquid was concentrated under a reduced pressure and dissolved in chloroform. The organic layer was washed with saturated brine, dried over anhydrous sodium sulfate and concentrated under a reduced pressure. The obtained residue (1.53 g) was dissolved in ethanol (6 mL), and then sodium ethoxide (510 mg, 7.5 mmol) was added, followed by heating under reflux for 3 hours. The reaction liquid was concentrated under a reduced pressure, and the obtained residue was dissolved in ethyl acetate. The organic layer was washed with saturated brine, dried over anhydrous sodium sulfate and concentrated under a reduced pressure. The obtained residue was purified by using silica gel chromatography (chloroform:methanol=100:1→50:1) to give tert-butyl 4-[4-amino-5-(ethoxycarbonyl)-1H-pyrrol-3-yl]piperidine-1-carboxylate (466 mg, 46.0%) as a pale yellow amorphous.

後処理

  1. customThe reaction liquid
  2. concentrationwas concentrated under a reduced pressure
  3. dissolutiondissolved in chloroform
  4. washThe organic layer was washed with saturated brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationconcentrated under a reduced pressure
  7. dissolutionThe obtained residue (1.53 g) was dissolved in ethanol (6 mL)
  8. temperatureby heating
  9. temperatureunder reflux for 3 hours
  10. customThe reaction liquid
  11. concentrationwas concentrated under a reduced pressure
  12. dissolutionthe obtained residue was dissolved in ethyl acetate
  13. washThe organic layer was washed with saturated brine
  14. dry with materialdried over anhydrous sodium sulfate
  15. concentrationconcentrated under a reduced pressure
  16. customThe obtained residue was purified

出典と根拠

ORDレコード
ord-2599562d154e47768b1e1de0c5f93256
出典データセット
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08765771B2

反応ノート

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