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Sodium Hydroxide → 3-(4-Amino-3-methoxy-phenyl)-3-(3,4,5-trimethoxy-phenyl)-acrylonitrile

HRID 971004
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HRID 971004 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:12]([C:16]2[CH:21]=[C:20]([O:22][CH3:23])[C:19]([O:24][CH3:25])=[C:18]([O:26][CH3:27])[CH:17]=2)=[CH:13][C:14]#[N:15])[CH:6]=[CH:7][C:8]=1[N+:9]([O-])=O.O.O.[Sn](Cl)(Cl)(Cl)Cl.[OH-].[Na+]>C(O)C>[NH2:9][C:8]1[CH:7]=[CH:6][C:5]([C:12]([C:16]2[CH:21]=[C:20]([O:22][CH3:23])[C:19]([O:24][CH3:25])=[C:18]([O:26][CH3:27])[CH:17]=2)=[CH:13][C:14]#[N:15])=[CH:4][C:3]=1[O:2][CH3:1]
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참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 692040173-(3-Methoxy-4-nitro-phenyl)-3-(3,4,5-trimethoxy-phenyl)-acrylonitrileHCID 85782573Tin tetrachloride dihydrate

생성물 1

HCID 692050643-(4-Amino-3-methoxy-phenyl)-3-(3,4,5-trimethoxy-phenyl)-acrylonitrile수율 49%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
70 °C

실험 절차

A suspension of 3-(3-methoxy-4-nitro-phenyl)-3-(3,4,5-trimethoxy-phenyl)-acrylonitrile (0.9 g, 2.4 mmol) and tin chloride dihydrate (4.0 g, 17.7 mmol) in ethanol (25 mL) was heated at 70° C. for 1 h. The mixture was cooled and poured into ice (200 mL). The pH was made strongly alkaline by the addition of ION NaOH. The mixture was extracted with EtOAc (5×50 mL) and the combined organic extracts were washed with water (40 mL), brine (40 mL), and dried (MgSO4). Solvent was removed and the residue was purified by flash chromatography (silica gel, Hexane:EtOAc 1:1) to afford mixture isomers of 3-(4-amino-3-methoxy-phenyl)-3-(3,4,5-trimethoxy-phenyl)-acrylonitrile (0.4 g, 42%) as a yellow solid: mp 123-125° C.; 1H NMR (CDCl3) δ 7.05-6.53 (m, 5H), 5.56(5.43) (s, 1H), 4.12 (s, 2H), 3.91-3.81 (m, 12H); 13C NMR (CDCl3) δ 163.19, 163.09, 152.99, 152.93, 146.63, 139.82, 138.74, 135.43, 132.66, 128.33, 126.35, 124.12, 118.96, 113.76, 113.74, 111.99, 110.22, 107.35, 106.42, 91.14, 90.52, 60.94, 56.28, 56.25, 55.74, 55.59; Anal Calcd for C19H20N2O4: C, 67.05; H, 5.92; N, 8.23. Found: c, 66.92; H, 5.76; N, 8.10.

후처리

  1. temperatureThe mixture was cooled
  2. extractionThe mixture was extracted with EtOAc (5×50 mL)
  3. washthe combined organic extracts were washed with water (40 mL), brine (40 mL)
  4. dry with materialdried (MgSO4)
  5. customSolvent was removed
  6. customthe residue was purified by flash chromatography (silica gel, Hexane:EtOAc 1:1)

출처 및 근거

ORD 기록
ord-03ffd68ae94048cc973ac7bebc7b15dc
출처 데이터셋
uspto-grants-2007_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07312241B2

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