Methyl 1-benzyl-4-methylpiperidin-3-yl-carbamate → 1-Benzyl-4-methylpiperidin-3-amine

HRID 1506191ノート

反応式

HRID 1506191 の反応式
[CH2:1]([N:8]1[CH2:13][CH2:12][CH:11]([CH3:14])[CH:10]([NH:15]C(=O)OC)[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1>Cl>[CH2:1]([N:8]1[CH2:13][CH2:12][CH:11]([CH3:14])[CH:10]([NH2:15])[CH2:9]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

3

反応物 1

HCID 53396489Methyl 1-benzyl-4-methylpiperidin-3-yl-carbamate

生成物 1

HCID 545937521-Benzyl-4-methylpiperidin-3-amine

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

Crude methyl rac-(3R,4R)-1-benzyl-4-methylpiperidin-3-ylcarbamate (2.3 g) in concentrated hydrochloric acid (15 mL) was refluxed for one day under heating and allowed to cool to room temperature. The hydrochloric acid was removed under reduced pressure, and the reaction mixture was partitioned between chloroform and saturated aqueous sodium chloride. The aqueous layer was basified with saturated aqueous sodium carbonate and extracted with ethyl acetate twice, and the organic layers were combined, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The resulting brown oil (4.94 g) containing the title compound was used for the next step without further purification.

後処理

  1. temperatureunder heating
  2. customThe hydrochloric acid was removed under reduced pressure
  3. customthe reaction mixture was partitioned between chloroform and saturated aqueous sodium chloride
  4. extractionextracted with ethyl acetate twice
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationconcentrated under reduced pressure
  7. additionThe resulting brown oil (4.94 g) containing the title compound
  8. customwas used for the next step without further purification

出典と根拠

ORDレコード
ord-589fcfe46d5b4d5090fc4ce70ae4beee
出典データセット
uspto-grants-2015_12
特許番号
US09216999B2

反応ノート

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