Acetone → HCID 178482503, 화합물

HRID 67726

반응식

HRID 67726 반응식
[CH3:1][NH:2][C:3](=[S:6])[NH:4][NH2:5].CC(C)=O.N1[CH:16]=[CH:15][CH:14]=CC=1.[C:17](Cl)(=[O:22])[C:18]([CH3:21])([CH3:20])[CH3:19]>O>[CH3:1][NH:2][C:3]1[S:6][C:15]([CH3:14])([CH3:16])[N:5]([C:17](=[O:22])[C:18]([CH3:21])([CH3:20])[CH3:19])[N:4]=1

참가 물질

6

반응물 4

HCID 180AcetoneHCID 1049PyridineHCID 62493Pivaloyl chlorideHCID 2723853N-Methylhydrazinecarbothioamide

생성물 1

HCID 178482503HCID 178482503, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A 52.5 g. portion of 4-methylthiosemicarbazide was suspended and partially dissolved in 250 ml. of acetone, and 39.5 g. of pyridine was added. The mixture was stirred for 15 minutes at ambient temperature, and then 60.5 g. of pivaloyl chloride was added slowly while the temperature of the reaction mixture was held at 20°-25°. The mixture was stirred at ambient temperature for 3 hours after the addition, and then 200 ml. of water was added. The reaction mixture was filtered, and the filter cake was washed with 100 ml. of nitromethane and vacuum dried at 50° to obtain 91.4 g. of the desired intermediate product, m.p. 162°-164°.

후처리

  1. dissolutionpartially dissolved in 250 ml
  2. customwas held at 20°-25°
  3. stirringThe mixture was stirred at ambient temperature for 3 hours
  4. additionafter the addition
  5. filtrationThe reaction mixture was filtered
  6. washthe filter cake was washed with 100 ml
  7. dry with materialof nitromethane and vacuum dried at 50°
  8. customto obtain 91.4 g

출처 및 근거

ORD 기록
ord-4b7df4c1a3284005a4e7170acdd589a1
출처 데이터셋
uspto-grants-1982_08
특허 번호
US04346225

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