Acetic Acid → 4-amino-6-(1-cyclopropylethyl)-5-oxo-3-thioxo-tetrahydro-1,2,4-(2H,4H)-triazine

HRID 231390

반응식

HRID 231390 반응식
[OH-].[Na+].[NH2:3][NH:4][C:5]([NH:7][NH2:8])=[S:6].[CH2:9]([OH:19])[CH2:10][CH2:11][CH2:12][CH2:13][CH2:14]CCCC.[C:20](O)(=O)C>O>[NH2:3][N:4]1[C:9](=[O:19])[CH:10]([CH:11]([CH:12]2[CH2:13][CH2:14]2)[CH3:20])[NH:8][NH:7][C:5]1=[S:6]

참가 물질

6

반응물 4

HCID 176Acetic AcidHCID 81741-DecanolHCID 14798Sodium HydroxideHCID 2724189Thiocarbohydrazide

생성물 1

HCID 200323464-amino-6-(1-cyclopropylethyl)-5-oxo-3-thioxo-tetrahydro-1,2,4-(2H,4H)-triazine

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
70 °C

실험 절차

882 g (4.14 mols) of 4-(cyclopropyl-methyl-methylene)-N-methylrhodanine (as an E/Z mixture) are introduced into a solution of 712 g (17.8 mols) of sodium hydroxide in 4.4 l of water. After the addition of 7 ml of alkylaryl polyglycol ether, the mixture is stirred at 70° C. until complete dissolution occurs (about 16 hours). 438 g (4.14 mols) of thiocarbohydrazide and 115 ml of 1-decanol are then added, the mixture is stirred for one hour at 70° C., and 1525 ml of acetic acid are rapidly added dropwise, causing the reaction product to precipitate. The mixture is stirred at 80° C. for a further 2 hours, allowed to cool to room temperature and the precipitate is filtered off with suction, washed several times with water and also with petroleum ether and dried at 70° C. 725 g (82.6% of theory) of the above compound of melting point 142°-143° C. are obtained.

후처리

  1. custom(about 16 hours)
  2. stirringthe mixture is stirred for one hour at 70° C.
  3. customto precipitate
  4. stirringThe mixture is stirred at 80° C. for a further 2 hours
  5. temperatureto cool to room temperature
  6. filtrationthe precipitate is filtered off with suction
  7. washwashed several times with water
  8. dry with materialalso with petroleum ether and dried at 70° C
  9. custom725 g (82.6% of theory) of the above compound of melting point 142°-143° C. are obtained

출처 및 근거

ORD 기록
ord-ed94ae41352b495ba92f8bf3ddc675ad
출처 데이터셋
uspto-grants-1989_07
특허 번호
US04846881

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