Acetic Anhydride → HCID 67447123、化合物

HRID 2368082ノート

反応式

HRID 2368082 の反応式
[NH2:1][CH:2]([CH3:18])[CH2:3][CH2:4][CH:5]1[CH2:10][CH2:9][N:8]([C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])[CH2:7][CH2:6]1.[C:19](OC(=O)C)(=[O:21])[CH3:20]>C(OCC)(=O)C>[C:19]([NH:1][CH:2]([CH3:18])[CH2:3][CH2:4][CH:5]1[CH2:10][CH2:9][N:8]([C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])[CH2:7][CH2:6]1)(=[O:21])[CH3:20]

参加物

4

反応物 2

HCID 7918Acetic AnhydrideHCID 575174851344684-60-1

生成物 1

HCID 67447123HCID 67447123、化合物収率 63.6%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

A solution of tert-butyl 4-(3-aminobutyl)piperidine-1-carboxylate (3.58 g) and acetic anhydride (4.13 g) in ethyl acetate (100 mL) was heated under reflux for 3 hr. The reaction mixture was allowed to cool to room temperature, washed with aqueous citric acid solution and saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure and the residue was purified by silica gel column chromatography (hexane/ethyl acetate) to give the title compound (2.65 g).

後処理

  1. temperatureunder reflux for 3 hr
  2. washwashed with aqueous citric acid solution and saturated brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customThe solvent was evaporated under reduced pressure
  5. customthe residue was purified by silica gel column chromatography (hexane/ethyl acetate)

出典と根拠

ORDレコード
ord-4c3c77ae453046f5aca65df0ecc565ba
出典データセット
uspto-grants-2014_04
特許番号
US08703758B2

反応ノート

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