1H-1,2,4-Triazole → HCID 23349974, 화합물

HRID 2058197노트

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HRID 2058197 반응식
[NH:1]1[CH:5]=[N:4][CH:3]=[N:2]1.Br[CH:7]([O:15][C:16]1[CH:21]=[CH:20][C:19]([Cl:22])=[CH:18][C:17]=1[Cl:23])[C:8](=[O:14])[C:9]([O:12][CH3:13])([CH3:11])[CH3:10].N12CCCCC1C=NCCC2>CC(C)=O>[Cl:23][C:17]1[CH:18]=[C:19]([Cl:22])[CH:20]=[CH:21][C:16]=1[O:15][CH:7]([N:1]1[CH:5]=[N:4][CH:3]=[N:2]1)[C:8](=[O:14])[C:9]([O:12][CH3:13])([CH3:11])[CH3:10]

참가 물질

5

반응물 3

HCID 92571H-1,2,4-TriazoleHCID 3141121,5-Diazabicyclo(5,4,0)undec-5-eneHCID 23349975HCID 23349975, 화합물

생성물 1

HCID 23349974HCID 23349974, 화합물수율 63.8%

시약·촉매·용매 1

HCID 180Acetone용매

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온도
0 °C

실험 절차

1H-1,2,4-Triazole (2.83 g, 0.041 mole) was added to a stirred solution of 14.6 g (0.041 mole) of 1-bromo-1-(2,4-dichlorophenoxy)-3-methoxy-3-methyl-2-butanone in 100 ml. of acetone at -10° C. To the resulting mixture, 6.09 g (0.041 mole) of 1,5-diazabicyclo[5.4.0]-undec-5-ene was added at a rate to maintain the temperature of the mixture below -5° C. After the addition was complete, the mixture was stirred an additional 30 minutes at 0° C. Then the solvent was evaporated off, the residue taken up in 300 ml. diethyl ether, and the resulting mixture extracted with water. The organic phase was dried using MgSO4 and the solvent evaporated. The residual yellow oil (13 g) was stirred for several minutes with boiling hexane, then filtered to remove insoluble material. Upon cooling the filtrate, 9.0 g (63.8% yield) of 1-(2,4-dichlorophenoxy)-1-(1H- 1,2,4-triazol-1-yl)-3-methoxy-3-methyl-2-butanone, m.p. 53°-54° C., was obtained.

후처리

  1. customat -10° C
  2. temperatureto maintain the temperature of the mixture below -5° C
  3. additionAfter the addition
  4. customThen the solvent was evaporated off
  5. extractiondiethyl ether, and the resulting mixture extracted with water
  6. customThe organic phase was dried
  7. customthe solvent evaporated
  8. stirringThe residual yellow oil (13 g) was stirred for several minutes with boiling hexane
  9. filtrationfiltered
  10. customto remove insoluble material

출처 및 근거

ORD 기록
ord-513187510f3541ad984f7e847c02f20b
출처 데이터셋
uspto-grants-1980_07
특허 번호
US04215127

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