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]>O.C(O)C>[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 24 ml of water and 24 ml of ethanol, 11.6 g of 2-amino-5-mercapto-1,3,4-thiadiazole and 3.8 g of sodium hydroxide were dissolved, 14.0 g of 1-bromohexane was added to this solution, and the mixture was heated to 70°-80° C. and stirred for 3 hours. After cooling, water was added and the mixture was filtered. The residue was washed with water, dried under reduced pressure, and recrystallized from an ethanol/n-hexane (1:1) mixture. Thus 14.5 g of 2-amino-5-hexylthio-1,3,4-thiadiazole was obtained. m.p. 113°-115° C. Yield 77%.
後処理
- temperaturethe mixture was heated to 70°-80° C.
- temperatureAfter cooling
- filtrationthe mixture was filtered
- washThe residue was washed with water
- customdried under reduced pressure
- customrecrystallized from an ethanol/n-hexane (1:1) mixture
出典と根拠
- ORDレコード
- ord-6432914c090d4f8787e299adb34c0060
- 出典データセット
- uspto-grants-1988_05
- 特許番号
- US04742063
反応ノート
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