Morpholine → 4-(4-Bromo-1,3-thiazol-2-yl)morpholine
반응식
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]=1참가 물질
4
실험 절차
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.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-232160f89dfd47b7a44bd470fa2c75fb
- 출처 데이터셋
- uspto-grants-2014_02
- 특허 번호
- US08658637B2
반응 노트
불러오는 중…