Morpholine → 4-(3-Butyn-1-yl)morpholine
反応式
[CH2:1](OS(C)(=O)=O)[CH2:2][C:3]#[CH:4].[NH:10]1[CH2:15][CH2:14][O:13][CH2:12][CH2:11]1>CCOCC>[CH2:1]([N:10]1[CH2:15][CH2:14][O:13][CH2:12][CH2:11]1)[CH2:2][C:3]#[CH:4]参加物
4
反応条件
- 温度
- 100 °C
実験手順
A mixture of methanesulfonic acid but-3-ynyl ester (10.1 g, 68 mmol) and morpholine (12.5 mL, 143 mmol) was heated to 100° C. for 1 h. The mixture was diluted with Et2O (50 mL) and filtered. The solid residue was discarded, and the mother liquor extracted with 3N HCl. The aqueous layer was basified with NaOH, and back-extracted into EtOAc. Drying (Na2SO4), concentration, and distillation (short-path, b.p.=130° C. at ˜5 mm Hg) game the title compound as a colorless oil. 1H NMR (CDCl3) δ 3.72 (t, 4H), 2.60 (t, 2H), 2.48 (t, 4H), 2.39 (td, 2H), 2.00 (t, 1H).
後処理
- filtrationfiltered
- extractionthe mother liquor extracted with 3N HCl
- extractionback-extracted into EtOAc
- customDrying
- concentration(Na2SO4), concentration, and distillation (short-path, b.p.=130° C. at ˜5 mm Hg) game the title compound as a colorless oil
出典と根拠
- ORDレコード
- ord-967a14a2464f4a9599f94f0c6669c5e3
- 出典データセット
- uspto-grants-2012_01
- 特許番号
- US08093229B2
反応ノート
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