tert-Butyl 4-(methoxy(methyl)carbamoyl)piperidine-1-carboxylate → Tert-butyl 4-benzoylpiperidine-1-carboxylate

HRID 2382191ノート

反応式

HRID 2382191 の反応式
CON(C)[C:4]([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)=[O:5].[C:20]1([Mg]Cl)[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1>C1COCC1>[C:4]([CH:6]1[CH2:7][CH2:8][N:9]([C:12]([O:14][C:15]([CH3:16])([CH3:17])[CH3:18])=[O:13])[CH2:10][CH2:11]1)(=[O:5])[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1

参加物

4

反応物 2

HCID 11065582tert-Butyl 4-(methoxy(methyl)carbamoyl)piperidine-1-carboxylateHCID 178478979HCID 178478979、化合物

生成物 1

HCID 10827307Tert-butyl 4-benzoylpiperidine-1-carboxylate収率 59%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of tert-butyl 4-(methoxy(methyl)carbamoyl)piperidine-1-carboxylate (8.0 g, 29.4 mmol) in THF (25 mL) was added PhMgCl (8.0 g, 58.8 mmol) dropwise at 0° C. After stirring at rt for 2 h, the reaction was quenched with ammonium chloride solution and extracted with ethyl acetate, dried over anhydrous sodium sulfate and concentrated under vacuum to afford tert-butyl 4-benzoylpiperidine-1-carboxylate (5 g, 59% yield) as a pale yellow solid which was used directly in the next step.

後処理

  1. customthe reaction was quenched with ammonium chloride solution
  2. extractionextracted with ethyl acetate
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationconcentrated under vacuum

出典と根拠

ORDレコード
ord-5aa05b7ef335495ab0f1d54e49721986
出典データセット
uspto-grants-2012_09
特許番号
US08258306B2

反応ノート

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