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Water → HCID 66961044, 화합물

HRID 1446612
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HRID 1446612 반응식
[H-].[Na+].[Cl:3][CH2:4][CH2:5][CH2:6][CH:7](P(OCC)(OCC)=O)[C:8]([O:10][C:11]([CH3:14])([CH3:13])[CH3:12])=[O:9].[F:23][C:24]1[CH:31]=[C:30]([N:32]2[CH:36]=[C:35]([CH3:37])[N:34]=[CH:33]2)[C:29]([O:38][CH3:39])=[CH:28][C:25]=1[CH:26]=O.O>C1COCC1.C(OCC)(=O)C>[Cl:3][CH2:4][CH2:5][CH2:6]/[C:7](=[CH:26]\[C:25]1[CH:28]=[C:29]([O:38][CH3:39])[C:30]([N:32]2[CH:36]=[C:35]([CH3:37])[N:34]=[CH:33]2)=[CH:31][C:24]=1[F:23])/[C:8]([O:10][C:11]([CH3:12])([CH3:13])[CH3:14])=[O:9]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 962WaterHCID 24758Sodium hydrideHCID 730140352-fluoro-5-methoxy-4-(4-methyl-1H-imidazol-1-yl)benzaldehydeHCID 86602480Tert-butyl 5-chloro-2-(diethoxyphosphoryl)valerate

생성물 1

HCID 66961044HCID 66961044, 화합물수율 106.5%

시약·촉매·용매 2

HCID 8028
Tetrahydrofuran
용매
2회
HCID 8857Ethyl Acetate용매

실험 절차

Sodium hydride (containing mineral oil at 40%, 0.68 g) was added to a solution of tert-butyl 5-chloro-2-(diethoxyphosphoryl)valerate (5.59 g) in THF (50 mL) in a nitrogen atmosphere at room temperature, and the reaction solution was stirred at room temperature for 30 minutes. A solution of 2-fluoro-5-methoxy-4-(4-methyl-1H-imidazol-1-yl)benzaldehyde (3.19 g) in THF (10 mL) was added to the reaction mixture, and the reaction solution was stirred at room temperature for 4 hours. Water and ethyl acetate were added to the reaction mixture and the organic layer was partitioned. The organic layer was washed with brine, and then dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The resulting residue was purified by silica gel chromatography (elution solvent:heptane-ethyl acetate system) to obtain tert-butyl (E)-5-chloro-2-(2-fluoro-5-methoxy-4-(4-methyl-1H-imidazol-1-yl)benzylidene)valerate (5.93 g). A solution of tert-butyl (E)-5-chloro-2-(2-fluoro-5-methoxy-4-(4-methyl-1H-imidazol-1-yl)benzylidene)valerate in trifluoroacetic acid (30 mL) was stirred while cooling with ice. After 2 hours, the reaction solution was concentrated under reduced pressure. Tert-butyl methyl ether was added to the resulting residue, and the resulting deposited solid was filtered to obtain 3 g of the title compound. Properties data of the compound are as follows.

후처리

  1. stirringthe reaction solution was stirred at room temperature for 4 hours
  2. customthe organic layer was partitioned
  3. washThe organic layer was washed with brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe resulting residue was purified by silica gel chromatography (elution solvent:heptane-ethyl acetate system)

출처 및 근거

ORD 기록
ord-cd7d972dcc924fbe82bdda57a2303eaf
출처 데이터셋
uspto-grants-2010_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07667041B2

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