N-bromobutanimide → 5-(Bromomethyl)-2-chloropyrimidine
反応式
[Cl:1][C:2]1[N:7]=[CH:6][C:5]([CH3:8])=[CH:4][N:3]=1.[Br:9]N1C(=O)CCC1=O>C(Cl)(Cl)(Cl)Cl.C(OOC(=O)C1C=CC=CC=1)(=O)C1C=CC=CC=1>[Br:9][CH2:8][C:5]1[CH:4]=[N:3][C:2]([Cl:1])=[N:7][CH:6]=1参加物
5
実験手順
In 30 ml of carbon tetrachloride, 1.04 g (8.13 mmol) of 2-chloro-5-methylpyrimidine was dissolved. To this solution, 1.73 g (9.75 mmol) of N-bromosuccinimide and 20 mg of benzoyl peroxide were added, followed by heating under reflux for 6 hours. After completion of the reaction, the reaction liquid was returned to room temperature, and concentrated under reduced pressure. Then, the residue was purified by silica gel column chromatography (hexane:ethyl acetate=3:1). Thus, 641 mg of 5-bromomethyl-2-chloropyrimidine was obtained (Percentage Yield: 380).
後処理
- temperatureby heating
- temperatureunder reflux for 6 hours
- customAfter completion of the reaction
- customthe reaction liquid
- customwas returned to room temperature
- concentrationconcentrated under reduced pressure
- customThen, the residue was purified by silica gel column chromatography (hexane:ethyl acetate=3:1)
出典と根拠
- ORDレコード
- ord-a3f0733e5cc94ae0be0a6fe3549b84e2
- 出典データセット
- uspto-grants-2016_06
- 特許番号
- US09357776B2
反応ノート
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