Triethylamine → Methyl 2-methyl-4,5-dihydro-1,3-oxazole-4-carboxylate
反応式
[CH2:1](N(CC)CC)[CH3:2].CCl.[NH2:10][C@H:11]([C:14]([OH:16])=[O:15])[CH2:12][OH:13].Cl.[CH2:18](OC(=N)C)C>ClCCl>[CH3:1][C:2]1[O:13][CH2:12][CH:11]([C:14]([O:16][CH3:18])=[O:15])[N:10]=1参加物
5
実験手順
Triethylamine (5.86 g, 58.01 mmol) was added to a suspension of L-serine methyl hydrochloride (4.5 g, 29.03 mmol) and ethylacetimidate hydrochloride (4.3 g, 34.95 mmol) in dichloromethane (40 mL) at 0° C. over a period of 20 min. The mixture was then stirred at ambient temperature for 18 h. The suspension was filtered and washed with diethyl ether. The solid which precipitated from the filtrate was again filtered and washed with diethyl ether. The resulting filtrate was dried over anhydrous sodium sulfate and concentrated in vacuo to afford methyl 2-methyl-4,5-dihydrooxazole-4-carboxylate (3 g, 72%) as a liquid.
後処理
- filtrationThe suspension was filtered
- washwashed with diethyl ether
- customThe solid which precipitated from the filtrate
- filtrationwas again filtered
- washwashed with diethyl ether
- dry with materialThe resulting filtrate was dried over anhydrous sodium sulfate
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-5ba83008ff2e46b78f47f806272b42eb
- 出典データセット
- uspto-grants-2015_03
- 特許番号
- US08993574B2
反応ノート
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