Hydrochloric Acid → 4-methyl-5-(pyridin-3-yl)-4H-1,2,4-triazole-3-thiol

HRID 639830노트

반응식

HRID 639830 반응식
[C:1]([NH:9][NH2:10])(=O)[C:2]1[CH:7]=[CH:6][CH:5]=[N:4][CH:3]=1.[CH3:11][N:12]=[C:13]=[S:14].C([O-])(O)=O.[Na+].Cl>CC(O)C.O>[CH3:11][N:12]1[C:1]([C:2]2[CH:3]=[N:4][CH:5]=[CH:6][CH:7]=2)=[N:9][NH:10][C:13]1=[S:14]

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 11112Nicotinic acid, hydrazideHCID 11167Methyl isothiocyanateHCID 516892Sodium Bicarbonate

생성물 1

HCID 7575824-methyl-5-(pyridin-3-yl)-4H-1,2,4-triazole-3-thiol

시약·촉매·용매 2

HCID 962Water용매HCID 3776Isopropanol용매

반응 조건

온도
70 °C

실험 절차

Nicotinohydrazide (10 g, 73 mmol) and methyl isothiocyanate (5.6 g, 76 mmol) were mixed in 2-propanol (150 ml) and heated to 70° C. o.n. The reaction was cooled to r.t. and evaporated to dryness. H2O (180 mL) and NaHCO3 (12.8 g, 152 mmol) were added to the residue and the mixture was refluxed o.n. The reaction mixture was cooled to r.t., acidified with concentrated HCl and the title compound, 13.1 g (93%), was collected by filtration. LC-MS (M++1): 193

후처리

  1. temperatureThe reaction was cooled to r.t.
  2. customevaporated to dryness
  3. temperaturethe mixture was refluxed o.n
  4. temperatureThe reaction mixture was cooled to r.t.
  5. filtrationthe title compound, 13.1 g (93%), was collected by filtration

출처 및 근거

ORD 기록
ord-6bdeeec6ea7f4e14b5c0781491d9c896
출처 데이터셋
uspto-grants-2010_04
특허 번호
US07691892B2

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