1-Bromohexane → Sbb043676
反応式
[NH2:1][C:2]1[S:3][C:4]([SH:7])=[N:5][N:6]=1.[OH-].[Na+].Br[CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH3:16]>C(O)C.O>[NH2:1][C:2]1[S:3][C:4]([S:7][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH3:16])=[N:5][N:6]=1参加物
6
実験手順
In 190 ml of ethanol and 240 ml of water, 81.5 g of 2-amino-5-mercapto-1,3,4-thiadiazole and 26.9 g of sodium hydroxide were added. To this solution, 99 g of 1-bromohexane was added and the resulting mixture was warmed to 60°~70° C. and stirred for 2 hours. After cooling, water was added to the reaction mixture, and the resulting solution was filtered. The residue was washed with water and dried under reduced pressure. The dried residue was recrystallized from an ethanol/hexane mixture, and thus 100.5 g of 2-amino-5-hexylthio-1,3,4-thiadiazole was obtained. m.p. 113°~115° C. Yield 77%.
後処理
- temperaturethe resulting mixture was warmed to 60°~70° C.
- temperatureAfter cooling
- filtrationthe resulting solution was filtered
- washThe residue was washed with water
- customdried under reduced pressure
- customThe dried residue was recrystallized from an ethanol/hexane mixture
出典と根拠
- ORDレコード
- ord-5267acc46329413ca55d2359d49b20ee
- 出典データセット
- uspto-grants-1990_11
- 特許番号
- US04971971
反応ノート
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