Pyridine → HCID 14883432, 화합물

HRID 1710045노트

반응식

HRID 1710045 반응식
[CH3:1][N:2]([C:4]([NH:6][CH3:7])=[S:5])[NH2:3].N1C=CC=CC=1.[S:14]1[CH:18]=[CH:17][CH:16]=[C:15]1[C:19](Cl)=[O:20]>CCOCC>[CH3:1][N:2]([C:4]([NH:6][CH3:7])=[S:5])[NH:3][C:19]([C:15]1[S:14][CH:18]=[CH:17][CH:16]=1)=[O:20]

참가 물질

5

반응물 3

HCID 1049Pyridine2회HCID 789282-Thiophenecarbonyl chlorideHCID 30341872,4-Dimethylthiosemicarbazide

생성물 1

HCID 14883432HCID 14883432, 화합물

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

To a stirred, room temperature, solution of 2,4-dimethylthiosemicarbazide (3.75 g, 3.15×10-2 mole) and pyridine (30 ml) was added dropwise 2-thiophenecarbonyl chloride (3.20 ml, 2.99×10-2 mole). After stirring overnight the pyridine was evaporated at reduced pressure and the concentrate was treated with H2O. The resulting semi-solid was extracted into ethyl acetate. The ethyl acetate extract was washed with saturated NaCl and subsequently dried over anhydrous Na2SO4. The drying agent was removed by filtration and the filtrate was evaporated at reduced pressure, leaving a slightly yellowish solid. This was treated with Et2O and the solid was collected by filtration affording a colorless powder: 4.7 g (68%), mp 176°-178° C.

후처리

  1. customwas evaporated at reduced pressure
  2. additionthe concentrate was treated with H2O
  3. extractionThe resulting semi-solid was extracted into ethyl acetate
  4. extractionThe ethyl acetate extract
  5. washwas washed with saturated NaCl
  6. dry with materialsubsequently dried over anhydrous Na2SO4
  7. customThe drying agent was removed by filtration
  8. customthe filtrate was evaporated at reduced pressure
  9. customleaving a slightly yellowish solid
  10. filtrationthe solid was collected by filtration
  11. customaffording a colorless powder

출처 및 근거

ORD 기록
ord-a6775e3fb1694d95b4c4a0ae53ce811a
출처 데이터셋
uspto-grants-1990_08
특허 번호
US04952593

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