Water → 4-(Methoxymethyl)piperidine
反応式
C(OC([N:8]1[CH2:13][CH2:12][CH:11]([CH2:14][OH:15])[CH2:10][CH2:9]1)=O)(C)(C)C.I[CH3:17].[H-].[Na+].O>CN(C=O)C>[CH3:17][O:15][CH2:14][CH:11]1[CH2:10][CH2:9][NH:8][CH2:13][CH2:12]1参加物
6
実験手順
To a solution of 0.1 g (0.46 mmol) of 1-t-butoxycarbonyl-4-hydroxymethylpiperidine and 0.1 mL (1.6 mmol) of iodomethane in 2.5 mL of DMF was added 0.022 g (0.92 mmol) of NaH (80% dispersion in mineral oil). After 2 h, 10 mL of H2O was added to the reaction mixture and it was extracted with ether. The combined organic fractions were washed with sat'd NaCl solution, dried over MgSO4, filtered and the filtrate was concentrated. The residue was purified by chromatography (silica, hexanes:ethyl acetate=4:1) to give the title compound.
後処理
- extractionwas extracted with ether
- washThe combined organic fractions were washed with sat'd NaCl solution
- dry with materialdried over MgSO4
- filtrationfiltered
- concentrationthe filtrate was concentrated
- customThe residue was purified by chromatography (silica, hexanes:ethyl acetate=4:1)
出典と根拠
- ORDレコード
- ord-dd9a48cb5ccc45a083443b7d4d19caec
- 出典データセット
- uspto-grants-2002_09
- 特許番号
- US06455548B2
反応ノート
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