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

HRID 1461700

반응식

HRID 1461700 반응식
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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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%).

후처리

  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%)

출처 및 근거

ORD 기록
ord-f235a3e4cf324df5b44a3d694eb1d139
출처 데이터셋
uspto-grants-1991_12
특허 번호
US05077295

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