3-(1,3-Benzodioxol-5-yl)prop-2-yn-1-ol → HCID 11608001、化合物
反応式
[O:1]1[C:5]2[CH:6]=[CH:7][C:8]([C:10]#[C:11][CH2:12][OH:13])=[CH:9][C:4]=2[O:3][CH2:2]1>C(Cl)Cl.O=[Mn]=O>[O:1]1[C:5]2[CH:6]=[CH:7][C:8]([C:10]#[C:11][CH:12]=[O:13])=[CH:9][C:4]=2[O:3][CH2:2]1参加物
4
実験手順
To a solution of 3-(1,3-benzodioxol-5-yl)prop-2-yn-1-ol (242 mg, 1.37 mmol, obtained as described in Nugent et al., 1987, J. Am. Chem. Soc., 109, 2788) in anhydrous DCM (12 mL) was added MnO2 (2.70 g, 31.1 mmol) portion wise over 2 h. The resulting mixture was stirred at rt for one additional hour, then filtered on a bed of Celite and the filtrates were evaporated under reduced pressure to give 123 mg (51%) of the title compound as a brown solid. HPLC, Rt: 2.76 min (purity: 98.9%). 1H NMR (CDCl3) δ: 9.37 (s, 1H), 7.18 (m, 1H), 7.00 (m, 1H), 6.82 (d, J=8.3 Hz, 1H), 6.03 (s, 2H).
後処理
- filtrationfiltered on a bed of Celite
- customthe filtrates were evaporated under reduced pressure
出典と根拠
- ORDレコード
- ord-8621e4d42ddc4b878576e4219ab31fc7
- 出典データセット
- uspto-grants-2011_07
- 特許番号
- US07973039B2
反応ノート
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