反応式
N#N.Cl[CH2:4][C:5]1[O:9][C:8]([C:10]2([CH3:15])[O:14][CH2:13][CH2:12][O:11]2)=[CH:7][CH:6]=1.[C-:16]#[N:17].[Na+].O>CS(C)=O>[CH3:15][C:10]1([C:8]2[O:9][C:5]([CH2:4][C:16]#[N:17])=[CH:6][CH:7]=2)[O:14][CH2:13][CH2:12][O:11]1参加物
6
反応条件
- 温度
- 80 °C
実験手順
In a flame dried round-bottomed flask equipped with a magnetic stir bar and under inert atmosphere (N2), a solution of 2-(5-chloromethyl-furan-2-yl)-2-methyl-[1,3]dioxolane (2.37 mg, 11.68 mmol) in DMSO (50 mL) was treated with sodium cyanide (2.29 g, 46.72 mmol) and the reaction mixture was stirred at 80° C. for 45 min. Water (100 mL) was added to the cooled reaction mixture and the product was extracted with EA (2×100 mL). The combined org. extracts were dried over MgSO4, filtered, and the solvents were removed under reduced pressure. Purification of the residue by FC (2:1 hept-EA) gave the title compound as a yellow oil. LC-MS-conditions 02: tR=0.83 min.
後処理
- extractionthe product was extracted with EA (2×100 mL)
- dry with materialextracts were dried over MgSO4
- filtrationfiltered
- customthe solvents were removed under reduced pressure
- customPurification of the residue by FC (2:1 hept-EA)
出典と根拠
- ORDレコード
- ord-5fa81411ec84419cbe2c6f18f280b559
- 出典データセット
- uspto-grants-2014_03
- 特許番号
- US08674111B2
関連ノート
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