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Hydrochloric Acid → 4-{[3-tert-butyl-5-(2-phenylethyl)-1H-pyrazol-1-yl]methyl}benzaldehyde

HRID 507954
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HRID 507954 반응식
CN1CCNCC1.COCCO[Al-]OCCOC.[Na+].[C:20]([C:24]1[CH:28]=[C:27]([CH2:29][CH2:30][C:31]2[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=2)[N:26]([CH2:37][C:38]2[CH:47]=[CH:46][C:41]([C:42](OC)=[O:43])=[CH:40][CH:39]=2)[N:25]=1)([CH3:23])([CH3:22])[CH3:21].Cl>>[C:20]([C:24]1[CH:28]=[C:27]([CH2:29][CH2:30][C:31]2[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=2)[N:26]([CH2:37][C:38]2[CH:47]=[CH:46][C:41]([CH:42]=[O:43])=[CH:40][CH:39]=2)[N:25]=1)([CH3:23])([CH3:21])[CH3:22]
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참가 물질

5

반응물 4

HCID 313Hydrochloric AcidHCID 531671-MethylpiperazineHCID 16689465Sodium dihydrobis(2-methoxyethyl)aluminateHCID 23157206methyl 4-{[3-tert-butyl-5-(2-phenylethyl)-1H-pyrazol-1-yl]methyl}benzoate

생성물 1

HCID 231574034-{[3-tert-butyl-5-(2-phenylethyl)-1H-pyrazol-1-yl]methyl}benzaldehyde수율 92.3%

실험 절차

1-Methylpiperazine (10.7 g, 107 mmol) was added dropwise to sodium dihydridobis(2-methoxyethoxy)aluminate (70% toluene solution, 25 g, 86.6 mmol) at 0° C. To the obtained solution was added methyl 4-{[3-tert-butyl-5-(2-phenylethyl)-1H-pyrazol-1-yl]methyl}benzoate (1.65 g, 4.38 mmol) at 0° C. by small portions, and the mixture was further stirred at the same temperature for 1 hr. The reaction mixture was poured into 2 M hydrochloric acid, and the mixture was extracted with ethyl acetate. The extract was dried over anhydrous magnesium sulfate, and concentrated under reduced pressure to give the title compound (1.40 g, yield 92%) as a yellow oil.

후처리

  1. extractionthe mixture was extracted with ethyl acetate
  2. dry with materialThe extract was dried over anhydrous magnesium sulfate
  3. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-bf88df4a9dc7441da5c7c4485b85c5c5
출처 데이터셋
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07786165B2

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