Morpholine → 4-(4-Bromo-1,3-thiazol-2-yl)morpholine
反応式
Br[C:2]1[S:3][CH:4]=[C:5]([Br:7])[N:6]=1.[NH:8]1[CH2:13][CH2:12][O:11][CH2:10][CH2:9]1>O>[Br:7][C:5]1[N:6]=[C:2]([N:8]2[CH2:13][CH2:12][O:11][CH2:10][CH2:9]2)[S:3][CH:4]=1参加物
4
実験手順
A solution of 2,4-dibromothiazole (500 mg, 2.06 mmol) in morpholine (4.0 mL, 22.3 mmol) was warmed at 50° C. in a sealed tube. After 16 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 was 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 using ethyl acetate in hexanes (0-30% gradient) to afford 458 mg (89%) of 4-(4-bromothiazol-2-yl)morpholine.
後処理
- extractionextracted with three 30 mL portions of diethyl ether
- washThe combined organic layers was 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
出典と根拠
- ORDレコード
- ord-232160f89dfd47b7a44bd470fa2c75fb
- 出典データセット
- uspto-grants-2014_02
- 特許番号
- US08658637B2
反応ノート
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