2-Chloroethanol → 4-bromo-1-(2-chloroethyl)-1H-pyrazole
반응식
[Br:1][C:2]1[CH:3]=[N:4][NH:5][CH:6]=1.[Cl:7][CH2:8][CH2:9]O.C1C=CC(P(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.CCOC(/N=N/C(OCC)=O)=O>C1COCC1>[Br:1][C:2]1[CH:3]=[N:4][N:5]([CH2:9][CH2:8][Cl:7])[CH:6]=1참가 물질
6
실험 절차
To a solution of 4-bromo-1H-pyrazole (5 g, 34.02 mmol), 2-chloroethanol (2.7 mL, 40.82 mmol) and PPh3 (10.71 g, 40.82 mmol) and in THF (68 mL) at 0° C. was added DEAD (6.4 mL, 40.8 mmol). The mixture was allowed to warm-up to room temperature and stirred overnight. It was then concentrated under reduced pressure, the residue was treated with ether and the resultant suspension was filtered. The filtrate was collected and concentrated under reduced pressure to afford the title compound 75 which was used in the next step without further purification. MS (m/z): 209.0 (M+H).
후처리
- concentrationIt was then concentrated under reduced pressure
- additionthe residue was treated with ether
- filtrationthe resultant suspension was filtered
- customThe filtrate was collected
- concentrationconcentrated under reduced pressure
출처 및 근거
- ORD 기록
- ord-64b58d274e2e4aa28813d026de0dee4f
- 출처 데이터셋
- uspto-grants-2014_09
- 특허 번호
- US08846927B2
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