Tert-butyl 4-hydroxypiperidine-1-carboxylate → HCID 66811027、化合物

HRID 1097824ノート

反応式

HRID 1097824 の反応式
[CH:1]1([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=2[N:13]=[C:14]=[O:15])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[C:16]([O:20][C:21]([N:23]1[CH2:28][CH2:27][CH:26]([OH:29])[CH2:25][CH2:24]1)=[O:22])([CH3:19])([CH3:18])[CH3:17]>CN(C=O)C>[C:16]([O:20][C:21]([N:23]1[CH2:28][CH2:27][CH:26]([O:29][C:14](=[O:15])[NH:13][C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[CH:1]2[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]2)[CH2:25][CH2:24]1)=[O:22])([CH3:19])([CH3:17])[CH3:18]

参加物

4

反応物 2

HCID 643502Tert-butyl 4-hydroxypiperidine-1-carboxylateHCID 574747361-Cyclohexyl-2-isocyanatobenzene

生成物 1

HCID 66811027HCID 66811027、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A solution of the product of step (a) (˜9.8 mmol) and 4-hydroxypiperidine-1-carboxylic acid tert-butyl ester (2.4 g, 11.8 mmol) in DMF (19.7 mL) was stirred at room temperature for 24 h and then the solvent was removed under reduced pressure. The resulting residue was dissolved in ethyl acetate (20 mL) and this mixture was washed with 1N hydrochloric acid (2×10 mL), 1N aqueous sodium hydroxide (2×10 mL) and brine (10 mL), and then dried (MgSO4), filtered and the solvent removed under reduced pressure. The resulting residue was purified by column chromatography to give the title compound.

後処理

  1. customthe solvent was removed under reduced pressure
  2. dissolutionThe resulting residue was dissolved in ethyl acetate (20 mL)
  3. washthis mixture was washed with 1N hydrochloric acid (2×10 mL), 1N aqueous sodium hydroxide (2×10 mL) and brine (10 mL)
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. customthe solvent removed under reduced pressure
  7. customThe resulting residue was purified by column chromatography

出典と根拠

ORDレコード
ord-665298230f0342e384a57da01b803082
出典データセット
uspto-grants-2012_03
特許番号
US08143277B2

反応ノート

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