反応式
[CH3:1][N+:2]([CH2:5][CH:6]([OH:11])[CH2:7][C:8]([OH:10])=[O:9])(C)[CH3:3].[Cl-].N12CCN(CC1)CC2>CN(C=O)C>[CH3:1][N:2]([CH2:5][C@H:6]([OH:11])[CH2:7][C:8]([OH:10])=[O:9])[CH3:3]参加物
反応条件
- 温度
- 125 °C
実験手順
L-carnitine chloride (1.5. g; 0.008 moles) and 1,4 diazabicyclo[2,2,2]octane (5.25 g; 0.05 moles) were dissolved in 50 cc of DMF at 80° C. The resulting solution was subsequently heated up to 125° C. for 2 hours. Upon reaction termination, the solution was cooled in an ice bath a 5° C. After about 2 hours the precipitate which formed consisting of the excess diazabicyclo octane and its N-methyl derivative was filtered off. DMF was distilled under vacuum and the residue dissolved in water and eluted on AMBERLITE IRA 402 resin activated in the OH-l form. The eluate having alkaline pH was shown to consist of diazabicyclo octane and its N-methyl derivative; L-norcarnitine which formed was retained on the resin and was eluted therefrom with 2N HCl.
後処理
- customUpon reaction termination
- temperaturethe solution was cooled in an ice bath a 5° C
- customAfter about 2 hours the precipitate which formed
- filtrationwas filtered off
- distillationDMF was distilled under vacuum
- dissolutionthe residue dissolved in water
- washeluted on AMBERLITE IRA 402 resin
出典と根拠
- ORDレコード
- ord-4b7a83338cdf4bc8aacd50edcdfc5d19
- 出典データセット
- uspto-grants-1986_07
- 特許番号
- US04599447
関連ノート
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