反応式
[CH:1]1([CH:7]2[CH2:12][CH2:11][CH:10]([C:13]([OH:15])=O)[CH2:9][CH2:8]2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.C(Cl)(=O)C(Cl)=O.Cl.[CH3:23][C:24]([NH:27][OH:28])([CH3:26])[CH3:25]>O1CCCC1.CN(C)C=O.[OH-].[Na+]>[CH:1]1([CH:7]2[CH2:8][CH2:9][CH:10]([C:13]([N:27]([C:24]([CH3:26])([CH3:25])[CH3:23])[OH:28])=[O:15])[CH2:11][CH2:12]2)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]1参加物
反応物 3
生成物 1
試薬・触媒・溶媒 3
実験手順
To a solution of 4-cyclohexyl-cyclohexanecarboxylic acid (1.47 g, 7 mmol) in 20 ml of tetrahydrofuran was added oxalyl chloride (0.67 ml, 7.7 mmol) and a few drops of dimethylformamide. After stirring for one hour, the reaction mixture was added dropwise into a cold (~0° C.), stirred solution of N-(1,1-dimethylethyl)hydroxylamine hydrochloride (1.75 g, 14 mmol) in 40 ml of 1N sodium hydroxide. The mixture was stirred for two hours, from 0° C. to room temperature and extracted three times with ethyl acetate. The combined ethyl acetate extracts were then washed twice with water, dried with anhydrous sodium sulfate and concentrated. Purification by flash chromatography provided 0.186 g of the 4-cyclohexyl-N-(1,1-dimethylethyl)-N-hydroxy-cyclohexane-carboxamide as a white solid (m.p. 119°-120° C.).
後処理
- additionthe reaction mixture was added dropwise into a cold (~0° C.)
- stirringThe mixture was stirred for two hours, from 0° C. to room temperature
- extractionextracted three times with ethyl acetate
- washThe combined ethyl acetate extracts were then washed twice with water
- dry with materialdried with anhydrous sodium sulfate
- concentrationconcentrated
- customPurification by flash chromatography
出典と根拠
- ORDレコード
- ord-81dccbcadc124a5a82208d0bc9af450a
- 出典データセット
- uspto-grants-1989_12
- 特許番号
- US04889874
関連ノート
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