Dichloromethane → 1-[(4-Methoxy)phenyl]-3-[E-2-(methoxycarbonyl)ethenyl]-1H-pyrazole

HRID 394810노트

반응식

HRID 394810 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([N:9]2[CH:13]=[CH:12][C:11](NCC(OC)=O)=[N:10]2)=[CH:5][CH:4]=1.C1(P(=[CH:39][C:40]([O:42][CH3:43])=[O:41])(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[CH2:44](Cl)Cl>>[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]([N:9]2[CH:13]=[CH:12][C:11](/[CH:44]=[CH:39]/[C:40]([O:42][CH3:43])=[O:41])=[N:10]2)=[CH:7][CH:8]=1

참가 물질

4

반응물 3

HCID 6344DichloromethaneHCID 17453Acetic acid, 2-(triphenylphosphoranylidene)-, methyl esterHCID 865879801-[(4-Methoxy)phenyl]-3-[(methoxycarbonyl)methylamino]-1H-pyrazole

생성물 1

HCID 865879821-[(4-Methoxy)phenyl]-3-[E-2-(methoxycarbonyl)ethenyl]-1H-pyrazole수율 83%

실험 절차

To a solution of 1-[(4-methoxy)phenyl]-3-(carboxaldehyde)-1H-pyrazole-5-[(2′-tert-butylaminosulfonyl-[1,1′]-biphen-4-yl)carboxyamide (1.30 g, 2.44 mmol) in 30 mL of methylene chloride was added methyl (triphenylphosphoranylidene)acetate (0.98 g, 2.92 mmol). The mixture was allowed to stir at ambient temperature for 18 h. The volatiles were removed in vacuo and the residue was purified by flash chromatography (elution with 1:1 ethyl acetate/hexane) to afford 1.2 g (83%) of the title compound. LRMS. (ES+): 589.1 (M+H)+.

후처리

  1. customThe volatiles were removed in vacuo
  2. customthe residue was purified by flash chromatography (elution with 1:1 ethyl acetate/hexane)

출처 및 근거

ORD 기록
ord-23d5a74a84a04143af9a884be99da5a1
출처 데이터셋
uspto-grants-2003_08
특허 번호
US06602895B2

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