Sulfuric Acid → HCID 178441961, 화합물

HRID 1065103

반응식

HRID 1065103 반응식
C(O[C:5](=[O:7])[CH3:6])(=O)C.C(C#N)(=O)[C:9]([CH3:12])([CH3:11])[CH3:10].S(=O)(=O)(O)O.[NH2:21][NH:22][C:23]([NH:25][NH2:26])=[S:24]>Cl>[NH2:26][N:25]1[C:5](=[O:7])[C:6]([C:9]([CH3:10])([CH3:11])[CH3:12])=[N:21][N:22]=[C:23]1[SH:24]

참가 물질

6

반응물 4

HCID 1118Sulfuric AcidHCID 7918Acetic AnhydrideHCID 945273,3-Dimethyl-2-oxobutanenitrileHCID 2724189Thiocarbohydrazide

생성물 1

HCID 178441961HCID 178441961, 화합물수율 97.1%

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

실험 절차

First 25.6 g (0.25 mol) of acetic anhydride and then 27.8 g (0.25 mol) of pivaloyl cyanide were introduced, in each case at room temperature, into 49.0 g (0.5 mol) of concentrated sulphuric acid, which had been initially introduced into the reaction vessel. After subsequently stirring this reaction mixture for 0.5 hour, it was stirred into a solution of 26.6 g (0.25 mol) of thiocarbohydrazide in 300 ml of 1 N HCl at 20°-30° C. When the addition had ended, the mixture was subsequently stirred at 50°-55° C. for a further 1.5 hours; after cooling, the reaction product which had precipitated was filtered off, washed with 200 ml of water and dried. 48.6 g (97% of theory) of 4-amino-6-tert.-butyl-3-mercapto-1,2,4-triazin-5(4H)-one (V) were obtained as colorless crystals of melting point 212°-214° C.; content according to a determination by gas chromatography >99 %. No further purification operations were necessary for subsequent reactions.

후처리

  1. additionhad been initially introduced into the reaction vessel
  2. additionWhen the addition
  3. stirringthe mixture was subsequently stirred at 50°-55° C. for a further 1.5 hours
  4. temperatureafter cooling
  5. customthe reaction product which had precipitated
  6. filtrationwas filtered off
  7. washwashed with 200 ml of water
  8. customdried

출처 및 근거

ORD 기록
ord-c49fc2677e874fb7b13f2a099cde28b2
출처 데이터셋
uspto-grants-1982_05
특허 번호
US04328340

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