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

HRID 1607539노트

반응식

HRID 1607539 반응식
[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

참가 물질

6

반응물 3

HCID 14798Sodium HydroxideHCID 202741-IodoheptaneHCID 178509208HCID 178509208, 화합물

생성물 1

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

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매2회

반응 조건

온도
60 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-784b8e925b354ad79fd2c17566b0ac03
출처 데이터셋
uspto-grants-1989_09
특허 번호
US04866064

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