反応式
C([Li])CCC.[CH:6]1([NH:9][C:10]([C:12]2[N:13]=[C:14]([CH:17]([CH3:19])[CH3:18])[O:15][CH:16]=2)=[O:11])[CH2:8][CH2:7]1.[C:20](=[O:22])=[O:21]>CCCCCC.O1CCCC1>[CH:6]1([NH:9][C:10]([C:12]2[N:13]=[C:14]([CH:17]([CH3:19])[CH3:18])[O:15][C:16]=2[C:20]([OH:22])=[O:21])=[O:11])[CH2:7][CH2:8]1参加物
実験手順
0.12 mol of n-butyllithium (80.0 ml of a 1.5 molar solution in hexane) was added dropwise to a solution of 10.4 g (0.054 mol) of 2-(1-methylethyl)-oxazole-4-carboxylic acid cyclopropylamide in 250 ml of tetrahydrofuran under a nitrogen atmosphere of -70° C. and stirring was carried out for 30 minutes at this temperature. Thereafter, the reaction mixture was poured onto 500 g of solid CO2 and was left to stand overnight. The mixture was evaporated down, the residue was taken up in 200 ml of water and 30 ml of 10% strength NaOH, the solution was extracted twice with diethyl ether and the aqueous phase was acidified to pH 2 with concentrated hydrochloric acid and extracted with ethyl acetate. The organic phase was dried with magnesium sulfate and the solvent was stripped off under reduced pressure. 10.4 g (81%) of 4-cyclopropylaminocarbonyl-2-(1-methylethyl)-oxazole-5-carboxylic acid were obtained as a white powder of melting point 109° -112° C.
後処理
- waitwas left
- waitto stand overnight
- customThe mixture was evaporated down
- extraction30 ml of 10% strength NaOH, the solution was extracted twice with diethyl ether
- extractionextracted with ethyl acetate
- dry with materialThe organic phase was dried with magnesium sulfate
出典と根拠
- ORDレコード
- ord-5bde1ae0489f4953b2b8cb2e36f8a10e
- 出典データセット
- uspto-grants-1995_01
- 特許番号
- US05378680
関連ノート
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