Hydrochloric Acid → (3-Cyclopropyl-1,2-oxazol-5-yl)methanamine
反応式
C(OC([NH:8][CH2:9][C:10]1[O:14][N:13]=[C:12]([CH:15]2[CH2:17][CH2:16]2)[CH:11]=1)=O)(C)(C)C.Cl>CO>[NH2:8][CH2:9][C:10]1[O:14][N:13]=[C:12]([CH:15]2[CH2:17][CH2:16]2)[CH:11]=1参加物
4
実験手順
Crude 5-(tert-butoxycarbonylaminomethyl)-3-cyclopropylisoxazole (Method 3) (37.4 g, 0.157 mol) and 3M hydrochloric acid (80 ml) in methanol (100 ml) was heated at 50° C. for 2 hours. The methanol was removed by evaporation and aqueous residue washed with DCM. The aqueous layer was adjusted to pH 12 by careful addition of 40% aqueous sodium hydroxide solution and then extracted with DCM (×4). The extracts were combined, washed with brine, then dried (Na2SO4) and the volatiles removed by evaporation to give the title compound (11.5 g, 53%) as oil.
後処理
- customThe methanol was removed by evaporation and aqueous residue
- washwashed with DCM
- additionThe aqueous layer was adjusted to pH 12 by careful addition of 40% aqueous sodium hydroxide solution
- extractionextracted with DCM (×4)
- washwashed with brine
- dry with materialdried (Na2SO4)
- customthe volatiles removed by evaporation
出典と根拠
- ORDレコード
- ord-c818c0c7bd1c4ffab309d7af90a8cc5b
- 出典データセット
- uspto-grants-2009_08
- 特許番号
- US07579349B2
反応ノート
読み込み中…