1-Bromoheptane → 1,3,4-Thiadiazole, 2-amino-5-(heptylthio)-

HRID 1073793

反応式

HRID 1073793 の反応式
[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][CH2:16][CH3:17]>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][CH2:16][CH3:17])=[N:5][N:6]=1

参加物

6

反応物 3

HCID 123691-BromoheptaneHCID 14798Sodium HydroxideHCID 178509208HCID 178509208、化合物

生成物 1

HCID 5344581,3,4-Thiadiazole, 2-amino-5-(heptylthio)-収率 82.5%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒2 回

反応条件

温度
60 °C

実験手順

In 185 ml of ethanol and 185 ml of water, 68.0 g of 2-amino-5-mercapto-1,3,4-thiadiazole and 22.4 g of sodium hydroxide were added. To this mixture, 84.6 g of 1-bromoheptane was added, and the resulting mixture was warmed to 60° C. and stirred for 2 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/hexane mixture. Thus 90.2 g of 2-amino-5-heptylthio-1,3,4-thiadiazole was obtained. m.p. 112°~113° C. Yield 78%.

後処理

  1. temperatureAfter cooling
  2. filtrationthe mixture was filtered
  3. washThe residue was washed with water
  4. customdried under reduced pressure
  5. customrecrystallized from an ethanol/hexane mixture

出典と根拠

ORDレコード
ord-3e39365279be437890d2df62cf84d2c9
出典データセット
uspto-grants-1990_11
特許番号
US04971971

関連ノート

読み込み中…