反応式
[C:1](Cl)(=[O:5])[C:2]([CH3:4])=[CH2:3].Cl.[NH2:8][C@H:9]([C:14]([NH2:16])=[O:15])[CH2:10][C:11](=[O:13])[NH2:12].C(OCC)C.C(=O)([O-])[O-].[K+].[K+]>CO.O>[C:1]([NH:16][C:14](=[O:15])[C@H:9]([CH2:10][C:11](=[O:13])[NH2:12])[NH2:8])(=[O:5])[C:2]([CH3:4])=[CH2:3]参加物
実験手順
A 11.3 ml portion of methacrylic acid chloride, 1 g of asparagineamide hydrochloride (mfd. by Kokusan Kagaku) and 50 ml of diethyl ether were put into a 300 ml capacity eggplant type flask and stirred on an ice bath. Next, 20 ml of saturated potassium carbonate aqueous solution was added dropwise thereto. Thereafter, this was stirred on an ice bath for 30 minutes and then at room temperature for 12 hours. Diethyl ether layer in the thus obtained reaction liquid was discarded, and the water layer was dissolved in 100 ml of methanol. After filtration, the filtrate was concentrated under a reduced pressure and fractionated by a silica gel column using methanol as the developing solvent. The thus obtained amide compound fraction was purified using an ion exchange resin (“Dynaion (trade name) PA 412” mfd. by Mitsubishi Kagaku) After concentration under a reduced pressure and subsequent drying under a reduced pressure, 0.43 g of colorless crystals were obtained.
後処理
- stirringThereafter, this was stirred on an ice bath for 30 minutes
- filtrationAfter filtration
- concentrationthe filtrate was concentrated under a reduced pressure
- customThe thus obtained amide compound fraction was purified
- concentrationAfter concentration under a reduced pressure
- customsubsequent drying under a reduced pressure
出典と根拠
- ORDレコード
- ord-2b77fb6cdb414d78b7f09e69d2abd348
- 出典データセット
- uspto-grants-2010_12
- 特許番号
- US07847047B2
関連ノート
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