Morpholine → 4-(1,3-Thiazol-2-yl)morpholine
反応式
Br[C:2]1[S:3][CH:4]=[CH:5][N:6]=1.[NH:7]1[CH2:12][CH2:11][O:10][CH2:9][CH2:8]1>O>[S:3]1[CH:4]=[CH:5][N:6]=[C:2]1[N:7]1[CH2:12][CH2:11][O:10][CH2:9][CH2:8]1参加物
4
実験手順
A solution of 2-bromothiazole (356 μL, 4.00 mmol) in morpholine (2.09 mL, 24.0 mmol) was warmed at 100° C. in a sealed tube. After 61 hours, the mixture was cooled to room temperature, diluted with 20 mL of water, and extracted with three 30 mL portions of diethyl ether. The combined organic layers were washed with five 30 mL portions of water, 30 mL of brine, dried over magnesium sulfate, filtered, and concentrated in vacuo. The residue was chromatographed over SiO2 (20-100% ethyl acetate in hexanes, gradient) to afford 513 mg (75%) of 4-thiazol-2-yl-morpholine.
後処理
- extractionextracted with three 30 mL portions of diethyl ether
- washThe combined organic layers were washed with five 30 mL portions of water, 30 mL of brine
- dry with materialdried over magnesium sulfate
- filtrationfiltered
- concentrationconcentrated in vacuo
- customThe residue was chromatographed over SiO2 (20-100% ethyl acetate in hexanes, gradient)
出典と根拠
- ORDレコード
- ord-5e6803b3a4184742bdd816b014b0bbdb
- 出典データセット
- uspto-grants-2014_02
- 特許番号
- US08658637B2
反応ノート
読み込み中…