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Hydrochloric Acid → Dimethyl 4,4'-((1E,1'E)-1,4-phenylenebis(ethene-2,1-diyl))dibenzoate

HRID 523138
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HRID 523138 반응식
C(OP([CH2:9][C:10]1[CH:19]=[CH:18][C:13]([C:14]([O:16][CH3:17])=[O:15])=[CH:12][CH:11]=1)(OCC)=O)C.[CH:20]1[C:25]([CH:26]=[O:27])=[CH:24][CH:23]=[C:22]([CH:28]=O)[CH:21]=1.[CH3:30][O-:31].[Na+].Cl>C1COCC1>[C:10]1(/[CH:9]=[CH:9]/[C:10]2[CH:11]=[CH:12][C:13]([C:14]([O:16][CH3:17])=[O:15])=[CH:18][CH:19]=2)[CH:19]=[CH:18][C:13](/[CH:14]=[CH:28]/[C:22]2[CH:21]=[CH:20][C:25]([C:26]([O:31][CH3:30])=[O:27])=[CH:24][CH:23]=2)=[CH:12][CH:11]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 12173TerephthalaldehydeHCID 10942334Sodium MethoxideHCID 10946061Methyl 4-(diethoxyphosphorylmethyl)benzoate

생성물 1

HCID 22725869Dimethyl 4,4'-((1E,1'E)-1,4-phenylenebis(ethene-2,1-diyl))dibenzoate수율 84%

시약·촉매·용매 1

HCID 8028
Tetrahydrofuran
용매
2회

실험 절차

A solution of Methyl 4-((diethoxyphosphoryl)methyl)benzoate (2.02 g, 7.05 mmol) and terepthaldehyde (0.462 g, 3.44 mmol) in THF (12 mL) was added to a suspension of NaOMe (1.12 g, 20.6 mmol) in THF (70 mL). The reaction was stirred under nitrogen for four hours and was then neutralized with 1M HCl. The resulting suspension was filtered, the collected solid was washed with THF, EtOH, and H2O, then allowed to dry under vacuum to give a yellow solid (1.15 g, 2.88 mmol, 84%). Characterization data matches literature. J. C. Sancho-García, et al., J. Phys. Chem. B, 109:4872-4880 (2005).

후처리

  1. filtrationThe resulting suspension was filtered
  2. washthe collected solid was washed with THF, EtOH, and H2O
  3. customto dry under vacuum

출처 및 근거

ORD 기록
ord-de1fcfb7084d46a5a7fc91c7c835bde8
출처 데이터셋
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09334304B2

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