Methanol → 3,5,6-Trichloro-2-methylthiopyrazine
反応式
[Cl:1][C:2]1[N:7]=[C:6]([Cl:8])[C:5]([Cl:9])=[N:4][C:3]=1Cl.[Na+].[SH-:12].O.[CH3:14]O>>[Cl:1][C:2]1[C:3]([S:12][CH3:14])=[N:4][C:5]([Cl:9])=[C:6]([Cl:8])[N:7]=1参加物
5
実験手順
A solution was prepared by dissolving 25 grams (0.115 mole) of tetrachloropyrazine in 300 milliliters of methanol. To this solution was added over a 90 minute period, a solution of 115 milliliters of ~1.0 molar sodium mercaptide in methanol. The temperature was maintained below 20° C during the addition. The reaction mixture was stirred at room temperature overnight and thereafter poured into 400 milliliters of water. The precipitate which formed was removed by filtration and recrystallized from hexane. The 3,5,6-trichloro-2-methylthiopyrazine product was recovered in a yield of 7.11 grams, 27 percent of theoretical, and melted at 45°-47° C.
後処理
- customA solution was prepared
- additionTo this solution was added over a 90 minute period
- temperatureThe temperature was maintained below 20° C during the addition
- customThe precipitate which formed
- customwas removed by filtration
- customrecrystallized from hexane
- customThe 3,5,6-trichloro-2-methylthiopyrazine product was recovered in a yield of 7.11 grams, 27 percent of theoretical, and melted at 45°-47° C.
出典と根拠
- ORDレコード
- ord-4414d70699e643b4bac9a2c312fea4da
- 出典データセット
- uspto-grants-1978_07
- 特許番号
- US04101546
反応ノート
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