Dimethylcarbamoyl Chloride → 1H-1,2,4-Triazole-1-carboxamide, 3-tert-butyl-N,N-dimethyl-5-(methylthio)-

HRID 1833561노트

반응식

HRID 1833561 반응식
[C:1]([C:5]1[NH:9][C:8]([S:10][CH3:11])=[N:7][N:6]=1)([CH3:4])([CH3:3])[CH3:2].[CH3:12][N:13]([CH3:17])[C:14](Cl)=[O:15]>N1C=CC=CC=1>[CH3:12][N:13]([CH3:17])[C:14]([N:7]1[C:8]([S:10][CH3:11])=[N:9][C:5]([C:1]([CH3:4])([CH3:2])[CH3:3])=[N:6]1)=[O:15]

참가 물질

4

반응물 2

HCID 6598Dimethylcarbamoyl ChlorideHCID 178503613HCID 178503613, 화합물

생성물 1

HCID 30492461H-1,2,4-Triazole-1-carboxamide, 3-tert-butyl-N,N-dimethyl-5-(methylthio)-

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

A solution of 57.6 g (0.338 mol) of 3-tert.butyl-5-methylthio-4H-1,2,4-triazole and 38g (0.355 mol) of dimethylcarbamyl chloride in 300 ml of pyridine was maintained at reflux temperature for 16 hrs. After the pyridine was removed at reduced pressure on the rotary evaporator, water was added followed by chloroform. The organic layer was washed with successive portions of dilute hydrochloric acid, water and brine then dried over Na2SO4. The solvent was removed in vacuo to give 75 g, nD26 1.5165 of an oil. Spectral properties agree with the structure

후처리

  1. temperatureat reflux temperature for 16 hrs
  2. customAfter the pyridine was removed at reduced pressure on the rotary evaporator, water
  3. additionwas added
  4. washThe organic layer was washed with successive portions of dilute hydrochloric acid, water and brine
  5. dry with materialthen dried over Na2SO4
  6. customThe solvent was removed in vacuo
  7. customto give 75 g

출처 및 근거

ORD 기록
ord-529082be42b9413abc067bead47ce636
출처 데이터셋
uspto-grants-1978_01
특허 번호
US04066774

반응 노트

불러오는 중…