反応式
[CH3:1][C:2]1([CH2:12][O:13]CC#C)[NH:6][C:5]2(CCC[CH2:8][CH2:7]2)[O:4][CH2:3]1.Cl>O>[NH2:6][C:2]([CH3:1])([CH2:3][O:4][CH2:5][C:7]#[CH:8])[CH2:12][OH:13]参加物
4
実験手順
3-Methyl-3-prop-2-ynyloxymethyl-1-oxa-4-aza-spiro[4.5]decane (1.83 g) in an aqueous solution of HCl (6N) (2.73 ml) were refluxed for 1 hr. The reaction mixture was cooled down to room temperature, diluted with water and extracted thrice with ethyl ether. The two layers were separated. The aqueous layer was concentrated under reduced pressure to yield 2-amino-2-methyl-3-prop-2-ynyloxy-propan-1-ol hydrochloric salt (1.205 g) as a white beige solid which was used as such in Stage 3 described below. 1H NMR (DMSO) δ ppm: 8.02 (3H, s br); 5.47 (1H, s br); 4.21 (2H, s); 3.54-3.49 (5H, m); 1.15 (3H, s).
後処理
- extractionextracted thrice with ethyl ether
- customThe two layers were separated
- concentrationThe aqueous layer was concentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-ae3bb24121ea4854a6d21cbb4a62e16d
- 出典データセット
- uspto-grants-2013_04
- 特許番号
- US08415272B2
関連ノート
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