6-(2-methylpropyl)piperidine-2,4-dione → HCID 66732004、化合物

HRID 1963109ノート

反応式

HRID 1963109 の反応式
[H-].[H-].[H-].[H-].[Li+].[Al+3].[CH2:7]([CH:11]1[NH:16][C:15](=O)[CH2:14][C:13](=[O:18])[CH2:12]1)[CH:8]([CH3:10])[CH3:9]>C1COCC1>[CH2:7]([CH:11]1[CH2:12][CH:13]([OH:18])[CH2:14][CH2:15][NH:16]1)[CH:8]([CH3:10])[CH3:9]

参加物

4

反応物 2

HCID 52466806-(2-methylpropyl)piperidine-2,4-dioneHCID 21226445Aluminium lithium hydride

生成物 1

HCID 66732004HCID 66732004、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a stirred ice cooled suspension of LAH (16.1 g, 0.414 mol) in THF (100 mL), a solution of 6-isobutyl-piperidine-2,4-dione (14.0 g, 0.083 mol) in THF (100 mL) was added dropwise under N2. The reaction mixture was warmed to room temperature and stirred under N2 for 48 h. The reaction mixture was cooled to 0° C. and quenched with water (16.1 mL), 1 N NaOH (16.1 mL) and water (16.1 mL). The reaction mixture was filtered and the solid was washed with hot THF (100 mL). The filtrate was concentrated to yield 2-isobutyl-piperidin-4-ol as a solid (9 g, crude).

後処理

  1. temperatureThe reaction mixture was cooled to 0° C.
  2. customquenched with water (16.1 mL), 1 N NaOH (16.1 mL) and water (16.1 mL)
  3. filtrationThe reaction mixture was filtered
  4. washthe solid was washed with hot THF (100 mL)
  5. concentrationThe filtrate was concentrated

出典と根拠

ORDレコード
ord-8dc02dea70b647bd93facac53becd429
出典データセット
uspto-grants-2013_04
特許番号
US08415378B2

反応ノート

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