Piperidine → 4-Methyl-1-(piperidin-1-YL)pentan-1-one

HRID 1912039

反応式

HRID 1912039 の反応式
[CH3:1][CH:2]([CH3:8])[CH2:3][CH2:4][C:5]([OH:7])=O.[NH:9]1[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10]1.C1C=CC2N(O)N=NC=2C=1.CCN=C=NCCCN(C)C.Cl>O.CN(C=O)C>[CH3:8][CH:2]([CH3:1])[CH2:3][CH2:4][C:5]([N:9]1[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10]1)=[O:7]

参加物

7

反応物 4

HCID 8082PiperidineHCID 12587Isocaproic acidHCID 757711-HydroxybenzotriazoleHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride

生成物 1

HCID 229808734-Methyl-1-(piperidin-1-YL)pentan-1-one

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回HCID 6228Dimethylformamide溶媒

実験手順

4-Methylvaleric acid (238 g) and DMF (833 mL) were mixed. After an addition of piperidine (233 mL), HOBt.H2O (361 g) and WSC.HCl (452 g) to the mixture at ice temperature, the resulting mixture was stirred at RT overnight. To the reaction was added water (1000 mL) at ice temperature and the resulting mixture was extracted with toluene (500 mL×2). The organic layer was washed with aqueous 10 w/v % sodium carbonate (500 mL+300 mL) and water (500 mL×2). The organic layer was concentrated in vacuo to give the title compound (414.29 g) as a crude product.

後処理

  1. extractionthe resulting mixture was extracted with toluene (500 mL×2)
  2. washThe organic layer was washed with aqueous 10 w/v % sodium carbonate (500 mL+300 mL) and water (500 mL×2)
  3. concentrationThe organic layer was concentrated in vacuo

出典と根拠

ORDレコード
ord-e6ac6957f0574262993407896860be3e
出典データセット
uspto-grants-2013_12
特許番号
US08604069B2

関連ノート

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