Propanoic acid, 2-bromo-2-methyl-, ethyl ester → 2-Amino-5,5-dimethyl-thiazol-4-one
反応式
[NH2:1][C:2]([NH2:4])=[S:3].Br[C:6]([CH3:13])([CH3:12])[C:7](OCC)=[O:8]>C(O)C>[CH3:12][C:6]1([CH3:13])[S:3][C:2](=[NH:4])[NH:1][C:7]1=[O:8]参加物
4
実験手順
A suspension of thiourea (19.0 g, 0.25 mole) in 150 ml of ethanol was heated under reflux until all of the thiourea had dissolved. Ethyl 2-bromo-isobutyrate (49.0 g, 0.25 mole) was then added over 10 minutes to the refluxing solution, after which time the solution was heated under reflux for six hours then allowed to stir at ambient temperature 36 hours. The solution was concentrated to dryness and the residue treated with water, then with aqueous NaHCO3 to adjust the pH to 7.0. The precipitated solid was collected by filtration, washed with water and dried to yield 5,5-dimethyl-2-iminothiazolidin-4-one: mp 252°-254° C.; 15.0 g (0.12 mole, 47%). Structure was confirmed by IR and NMR.
後処理
- temperaturewas heated
- dissolutionhad dissolved
- temperatureafter which time the solution was heated
- temperatureunder reflux for six hours
- concentrationThe solution was concentrated to dryness
- additionthe residue treated with water
- filtrationThe precipitated solid was collected by filtration
- washwashed with water
- customdried
出典と根拠
- ORDレコード
- ord-b8f0a2bc7c98474694d91484736c19de
- 出典データセット
- uspto-grants-1984_01
- 特許番号
- US04428948
反応ノート
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