Methanol → HCID 19019154、化合物
反応式
[Br:1][CH2:2][CH2:3][CH:4]1[O:8][C:7](C)(C)[O:6][C:5]1=[O:11].CC1C=CC(S(O)(=O)=O)=CC=1.O.CO>C1(C)C=CC=CC=1>[CH3:7][O:6][C:5](=[O:11])[CH:4]([OH:8])[CH2:3][CH2:2][Br:1]参加物
5
実験手順
To a solution of 5-(2-bromo-ethyl)-2,2-dimethyl-[1,3]dioxolan-4-one (synthesized as instructed in Tetrahedron Letters, 1997, 38, 28, 4935) (93 mg, 0.416 mmol) in toluene (0.5 mL) were added p-TsOH.H2O (8 mg, 0.0415 mmol) and methanol (0.5 mL), followed stirring overnight at room temperature. The solution was concentrated in a vacuum, diluted with dichloromethane and washed with an aqueous saturated sodium bicarbonate solution. The organic layer thus formed was dried over sodium sulfate and filtered. The filtrate was concentrated to produce 68 mg of the compound as an oil. 1H NMR (300 MHz, CDCl3) δ 1.98 (1H, m), 2.34 (1H, m), 2.96 (1H, d), 3.56 (2H, m), 3.82 (3H, s), 4.37 (1H, pentet).
後処理
- concentrationThe solution was concentrated in a vacuum
- additiondiluted with dichloromethane
- washwashed with an aqueous saturated sodium bicarbonate solution
- customThe organic layer thus formed
- dry with materialwas dried over sodium sulfate
- filtrationfiltered
- concentrationThe filtrate was concentrated
出典と根拠
- ORDレコード
- ord-855d9b29f33845d3b89d95972e9fc1b4
- 出典データセット
- uspto-grants-2015_05
- 特許番号
- US09034850B2
反応ノート
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