2-Chloroethanol → 4-bromo-1-(2-chloroethyl)-1H-pyrazole
反応式
[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]=1参加物
6
実験手順
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).
後処理
- 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
出典と根拠
- ORDレコード
- ord-64b58d274e2e4aa28813d026de0dee4f
- 出典データセット
- uspto-grants-2014_09
- 特許番号
- US08846927B2
反応ノート
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