Nitrogen → 3-(4-Hydroxybutyl)-1,8,8-trimethyl-3-azabicyclo-[3.2.1]octane-2,4-dione

HRID 1461700

反応式

HRID 1461700 の反応式
N#N.[CH3:3][C:4]1([CH3:15])[C:8]2([CH3:14])[C:9]([O:11][C:12](=[O:13])[CH:5]1[CH2:6][CH2:7]2)=O.[OH:16][CH2:17][CH2:18][CH2:19][CH2:20][NH2:21].C1(C)C=CC=CC=1>O>[OH:16][CH2:17][CH2:18][CH2:19][CH2:20][N:21]1[C:12](=[O:13])[CH:5]2[C:4]([CH3:3])([CH3:15])[C:8]([CH3:14])([CH2:7][CH2:6]2)[C:9]1=[O:11]

参加物

6

反応物 4

HCID 947NitrogenHCID 1140TolueneHCID 258684-Amino-1-butanolHCID 948341,8,8-Trimethyl-3-oxabicyclo[3.2.1]octane-2,4-dione

生成物 1

HCID 146490673-(4-Hydroxybutyl)-1,8,8-trimethyl-3-azabicyclo-[3.2.1]octane-2,4-dione

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a 125 ml round-bottomed flask equipped with Dean-Stark trap, condenser, and N2 inlet were added 5.35 g (29 mmol) of d-camphoric anhydride, 2.49 g (28 mmol) of 4-hydroxybutylamine, and 60 ml of toluene. The reaction was refluxed with separation of water for 20 hours. It was then cooled, concentrated to an oil, and the oil dissolved in ethyl acetate. The ethyl acetate solution was washed with 5% HCl, 5% NaOH, and brine, dried over sodium sulfate, and evaporated to an oil, 6.0 g (85%).

後処理

  1. temperatureIt was then cooled
  2. concentrationconcentrated to an oil
  3. dissolutionthe oil dissolved in ethyl acetate
  4. washThe ethyl acetate solution was washed with 5% HCl, 5% NaOH, and brine
  5. dry with materialdried over sodium sulfate
  6. customevaporated to an oil, 6.0 g (85%)

出典と根拠

ORDレコード
ord-f235a3e4cf324df5b44a3d694eb1d139
出典データセット
uspto-grants-1991_12
特許番号
US05077295

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