tert-Butyl methyl ether → ethyl 3-(bromoacetyl)-1-(3-chloropyridin-2-yl)-1H-pyrazole-5-carboxylate

HRID 1630661노트

반응식

HRID 1630661 반응식
[C:1]([C:4]1[CH:8]=[C:7]([C:9]([O:11][CH2:12][CH3:13])=[O:10])[N:6]([C:14]2[C:19]([Cl:20])=[CH:18][CH:17]=[CH:16][N:15]=2)[N:5]=1)(=[O:3])[CH3:2].O1CCOCC1.C(OC)(C)(C)C.[Br:33]Br>O>[Br:33][CH2:2][C:1]([C:4]1[CH:8]=[C:7]([C:9]([O:11][CH2:12][CH3:13])=[O:10])[N:6]([C:14]2[C:19]([Cl:20])=[CH:18][CH:17]=[CH:16][N:15]=2)[N:5]=1)=[O:3]

참가 물질

6

반응물 4

HCID 15413tert-Butyl methyl etherHCID 24408BromineHCID 312751,4-DioxaneHCID 66587473ethyl 3-acetyl-1-(3-chloropyridin-2-yl)-1H-pyrazole-5-carboxylate

생성물 1

HCID 86661386ethyl 3-(bromoacetyl)-1-(3-chloropyridin-2-yl)-1H-pyrazole-5-carboxylate

시약·촉매·용매 1

HCID 962Water용매

실험 절차

1.20 g (4.40 mmol) of ethyl 3-acetyl-1-(3-chloropyridin-2-yl)-1H-pyrazole-5-carboxylate were initially charged in in each case 30 ml of dioxane and methyl tert-butyl ether and 776 mg (4.85 mmol) of bromine were added dropwise at RT. The mixture was then stirred under reflux for 6 h. The reaction mixture was added to water, and the organic phase was separated off, dried over sodium sulphate and concentrated. The residue was recrystallized from methyl tert-butyl ether.

후처리

  1. additionwere added dropwise at RT
  2. temperatureunder reflux for 6 h
  3. customthe organic phase was separated off
  4. dry with materialdried over sodium sulphate
  5. concentrationconcentrated
  6. customThe residue was recrystallized from methyl tert-butyl ether

출처 및 근거

ORD 기록
ord-9378d0a888894f969763d0eaa51dcc3b
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08791139B2

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