Hydrogen Bromide → Carboxymethyl 5-amino-4-oxopentanoate hydrobromide
反応式
[BrH:1].C([NH:9][CH2:10][C:11](=[O:25])[CH2:12][CH2:13][C:14]([O:16][CH2:17][C:18]([O:20]C(C)(C)C)=[O:19])=[O:15])(OC(C)(C)C)=O>C(O)(=O)C>[BrH:1].[NH2:9][CH2:10][C:11](=[O:25])[CH2:12][CH2:13][C:14]([O:16][CH2:17][C:18]([OH:20])=[O:19])=[O:15]参加物
4
実験手順
A 30% solution of hydrogen bromide in acetic acid (12 mL) was added to the product of 1a (3.3 g; 9.5 mmol) cooled with an ice-water bath and stirred until the oil dissolved with evolution of gas. After stirring for 15 min, the mixture was triturated with hexane (4×20 mL) and diethyl ether (4×20 mL); the oil solidified to a tan powder. The residue was filtered and dried overnight in a drying pistol at ˜50° C. and 12 mm Hg. 4.44 g (92%) product was obtained (tan powder, mp 110-114° C. (dec.)).
後処理
- temperaturecooled with an ice-water bath
- dissolutiondissolved with evolution of gas
- stirringAfter stirring for 15 min
- customthe mixture was triturated with hexane (4×20 mL) and diethyl ether (4×20 mL)
- filtrationThe residue was filtered
- customdried overnight in a drying pistol at ˜50° C.
出典と根拠
- ORDレコード
- ord-e967cac021ed444685766933b4fc5d22
- 出典データセット
- uspto-grants-2016_02
- 特許番号
- US09249086B2
反応ノート
読み込み中…