4,5,6-Trichloro-2-methylpyrimidine → HCID 15003621、化合物
反応式
[CH3:1][O-:2].[Na+].[CH3:4][C:5]1[N:10]=[C:9](Cl)[C:8]([Cl:12])=[C:7]([Cl:13])[N:6]=1>C1COCC1>[Cl:13][C:7]1[C:8]([Cl:12])=[C:9]([O:2][CH3:1])[N:10]=[C:5]([CH3:4])[N:6]=1参加物
4
反応条件
- 温度
- 5 °C
実験手順
1.37 g of sodium methoxide are added to a solution of 5 g of 2-methyl-4,5,6-trichloropyrimidine in 41 ml of THF cooled to 5° C. in an ice bath. The ice bath is removed. The suspension is stirred at ambient temperature for 18 hours. The reaction medium is cooled to 5° C. in an ice bath. 20 ml of water and 100 ml of ethyl acetate are added. After settling out, the organic phase is dried over magnesium sulfate, filtered, and concentrated under reduced pressure so as to give 4.73 g of 4,5-dichloro-6-methoxy-2-methylpyrimidine in the form of a colorless oil which crystallizes, the characteristics of which are the following:
後処理
- customThe ice bath is removed
- temperatureThe reaction medium is cooled to 5° C. in an ice bath
- addition20 ml of water and 100 ml of ethyl acetate are added
- dry with materialthe organic phase is dried over magnesium sulfate
- filtrationfiltered
- concentrationconcentrated under reduced pressure so as
出典と根拠
- ORDレコード
- ord-9879af4a3e9f413faeb4d7b3182b496b
- 出典データセット
- uspto-grants-2015_09
- 特許番号
- US09133168B2
反応ノート
読み込み中…