Methanol → Tricyclo(3.3.1.13,7)dec-1-ylmethylamine
反応式
[C:1]12([C:11]([NH2:13])=O)[CH2:10][CH:5]3[CH2:6][CH:7]([CH2:9][CH:3]([CH2:4]3)[CH2:2]1)[CH2:8]2.S(C)C.CO>C1COCC1>[C:1]12([CH2:11][NH2:13])[CH2:8][CH:7]3[CH2:6][CH:5]([CH2:4][CH:3]([CH2:9]3)[CH2:2]1)[CH2:10]2参加物
5
実験手順
To a solution of admantane-1-carboxamide (2 g, 11.17 mmol) in THF (50 mL) was added BH3.Me2S (10.2 M, 3.4 mL, 34.7 mmol) under nitrogen. The mixture was heated at reflux overnight. The solution was cooled to rt. Methanol (20 mL) was added to the solution. The mixture was concentrated under vacuum to give crude product, which was purified by chromatography on silica gel to afford (1-adamantyl)methylamine (1.09 g, 59%). 1H NMR (CDCl3, 400 MHz): δ=1.44-1.96 (m, 15H), 2.30 (s, 2H).
後処理
- temperatureThe mixture was heated
- temperatureat reflux overnight
- concentrationThe mixture was concentrated under vacuum
- customto give crude product, which
- customwas purified by chromatography on silica gel
出典と根拠
- ORDレコード
- ord-6ea67caa19ef43d084cf1bbdb95ce0e3
- 出典データセット
- uspto-grants-2014_09
- 特許番号
- US08835426B2
反応ノート
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