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

HRID 1607539ノート

反応式

HRID 1607539 の反応式
[NH2:1][C:2]1[S:3][C:4]([SH:7])=[N:5][N:6]=1.[OH-].[Na+].I[CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH3:17]>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][CH2:16][CH3:17])=[N:5][N:6]=1

参加物

6

反応物 3

HCID 14798Sodium HydroxideHCID 202741-IodoheptaneHCID 178509208HCID 178509208、化合物

生成物 1

HCID 5344581,3,4-Thiadiazole, 2-amino-5-(heptylthio)-収率 78%

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 32 ml of water and 32 ml of ethanol, 27.2 g of 2-amino-5-mercapto-1,3,4-thiadiazole and 9.0 g of sodium hydroxide were added. To this solution, 45.2 g of 1-iodoheptane was added, and the mixture was stirred at 60° C. for 2 hours. After cooling, water was added to the mixture 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 36.1 g of 2-amino-5-heptylthio-1,3,4-thiadiazole was obtained.

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/n-hexane (1:1) mixture

出典と根拠

ORDレコード
ord-784b8e925b354ad79fd2c17566b0ac03
出典データセット
uspto-grants-1989_09
特許番号
US04866064

反応ノート

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