Diethylamine → Tetrahydrofuran
反応式
CC1C=CC(S([O:11][CH2:12][CH2:13][C:14]#[CH:15])(=O)=O)=CC=1.C([O-])([O-])=O.[K+].[K+].[CH2:22]([NH:24][CH2:25][CH3:26])[CH3:23]>C1COCC1>[CH2:22]([N:24]([CH2:25][CH3:26])[CH2:12][CH2:13][C:14]#[CH:15])[CH3:23].[CH2:14]1[CH2:15][O:11][CH2:12][CH2:13]1参加物
6
実験手順
A mixture of 3-butynyl 4-methylbenzenesulfonate (10 mL, 57 mmol), K2CO3 (7.9 g, 57 mmol), and diethylamine (23.5 mL, 228 mmol) in 100 mL of THF was heated to reflux for 31 hours, cooled to room temperature, and filtered. The filtrate was concentrated under vacuum at a distillation temperature of 60° C. to provide 11.2 g of a 53 wt % solution of the desired product in THF (5.9 g assay, 83% yield). 1H NMR (400 MHz, DMSO-d6) δ 0.93 (t, J=7.07 Hz, 6H) 2.21 (m, 2H) 2.44 (q, J=7.04 Hz, 4H) 2.55 (m, 2H) 2.72 (t, J=2.68 Hz, 1H).
後処理
- temperaturewas heated
- temperatureto reflux for 31 hours
- filtrationfiltered
- concentrationThe filtrate was concentrated under vacuum at a distillation temperature of 60° C.
出典と根拠
- ORDレコード
- ord-70b547921c8e48cf85b21fd40dd264fc
- 出典データセット
- uspto-grants-2009_02
- 特許番号
- US07491718B2
反応ノート
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