Morpholine → 4-(Pent-4-YN-1-YL)morpholine
反応式
I[CH2:2][CH2:3][CH2:4][C:5]#[CH:6].[NH:7]1[CH2:12][CH2:11][O:10][CH2:9][CH2:8]1>CCOCC>[CH2:2]([N:7]1[CH2:12][CH2:11][O:10][CH2:9][CH2:8]1)[CH2:3][CH2:4][C:5]#[CH:6]参加物
4
反応条件
- 温度
- 80 °C
実験手順
A mixture of 5-iodo-pent-1-yne (2.40 g, 12.3 mmol) and morpholine (2.70 g, 30.9 mmol) was heated to 80° C. for 15 min. The mixture was diluted with Et2O and filtered. The solid residue was discarded, and the mother liquor was extracted with 3N HCl. The aqueous layer was made basic with NaOH, and back-extracted into EtOAc. Drying (Na2SO4), and concentration gave the title compound as a pale orange oil. 1H NMR (CDCl3) δ 3.67 (t, 4H), 2.39 (m, 6H), 2.21 (td, 2H), 1.93 (t, 1H), 1.67 (quint., 2H).
後処理
- filtrationfiltered
- extractionthe mother liquor was extracted with 3N HCl
- extractionback-extracted into EtOAc
- customDrying
- concentration(Na2SO4), and concentration
出典と根拠
- ORDレコード
- ord-49350dfb8b9f49b7a299651d1b1938b8
- 出典データセット
- uspto-grants-2012_01
- 特許番号
- US08093229B2
反応ノート
読み込み中…