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Lithium hydroxide, monohydrate → tert-butyl(E)-5-chloro-2-{1-[3-fluoro-4-(4-methyl-1H-imidazol-1-yl)phenyl]methylidene}valerate

HRID 1436138
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HRID 1436138 반응식
[F:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][C:9]=1[N:10]1[CH:14]=[C:13]([CH3:15])[N:12]=[CH:11]1)[CH:5]=O.[Cl:16][CH2:17][CH2:18][CH2:19][CH:20](P(OCC)(OCC)=O)[C:21]([O:23][C:24]([CH3:27])([CH3:26])[CH3:25])=[O:22].O.[OH-].[Li+].O.C(=O)(O)[O-].[Na+]>C1COCC1.C(O)C>[Cl:16][CH2:17][CH2:18][CH2:19]/[C:20](=[CH:5]\[C:4]1[CH:7]=[CH:8][C:9]([N:10]2[CH:14]=[C:13]([CH3:15])[N:12]=[CH:11]2)=[C:2]([F:1])[CH:3]=1)/[C:21]([O:23][C:24]([CH3:27])([CH3:26])[CH3:25])=[O:22]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 168937Lithium hydroxide, monohydrateHCID 707008423-Fluoro-4-(4-methyl-1H-imidazol-1-yl)benzaldehydeHCID 86585896Sodium bicarbonate waterHCID 86602480Tert-butyl 5-chloro-2-(diethoxyphosphoryl)valerate

생성물 1

HCID 69004836tert-butyl(E)-5-chloro-2-{1-[3-fluoro-4-(4-methyl-1H-imidazol-1-yl)phenyl]methylidene}valerate수율 46.2%

시약·촉매·용매

2
HCID 702Ethanol용매HCID 8028Tetrahydrofuran용매

실험 절차

3-Fluoro-4-(4-methyl-1H-imidazol-1-yl)benzaldehyde (2.29 g) and tert-butyl 5-chloro-2-(diethoxyphosphoryl)valerate (3.68 g) were dissolved in a mixed solvent of THF (30 mL) and ethanol (10 mL). Lithium hydroxide monohydrate (1.41 g) was added to the reaction solution at room temperature, and the reaction solution was stirred at room temperature for 18 hours. Saturated sodium bicarbonate water was added to the reaction solution, followed by extraction with ethyl acetate. The resulting extract was dried over magnesium sulfate and then concentrated under reduced pressure. The residue was purified by silica gel column chromatography (elution solvent: heptane-ethyl acetate system), solidified with tert-butyl methyl ether and heptane, and separated by filtration to obtain 1.96 g of the title compound. The property values of the compound are as follows.

후처리

  1. extractionfollowed by extraction with ethyl acetate
  2. extractionThe resulting extract
  3. dry with materialwas dried over magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe residue was purified by silica gel column chromatography (elution solvent: heptane-ethyl acetate system)
  6. customseparated by filtration

출처 및 근거

ORD 기록
ord-e4245d1eb6c94ba9994356168e0a6688
출처 데이터셋
uspto-grants-2009_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07618960B2

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