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3-Methoxyaniline → HCID 21890102, 화합물

HRID 721600
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HRID 721600 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[O:13][CH3:14])[N:9]=[CH:8][CH:7]=[C:6]2[O:15][C:16]1[CH:26]=[CH:25][C:19]([O:20][CH2:21][C:22]([OH:24])=O)=[CH:18][CH:17]=1.CCN=C=NCCCN(C)C.Cl.C1C=CC2N(O)N=NC=2C=1.[CH3:49][O:50][C:51]1[CH:56]=[CH:55][CH:54]=[C:53]([NH2:57])[CH:52]=1.C(=O)([O-])O.[Na+]>C(Cl)(Cl)Cl.O>[CH3:49][O:50][C:51]1[CH:52]=[C:53]([NH:57][C:22](=[O:24])[CH2:21][O:20][C:19]2[CH:25]=[CH:26][C:16]([O:15][C:6]3[C:5]4[C:10](=[CH:11][C:12]([O:13][CH3:14])=[C:3]([O:2][CH3:1])[CH:4]=4)[N:9]=[CH:8][CH:7]=3)=[CH:17][CH:18]=2)[CH:54]=[CH:55][CH:56]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 5

HCID 108243-MethoxyanilineHCID 757711-HydroxybenzotriazoleHCID 516892Sodium BicarbonateHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 21890558HCID 21890558, 화합물

생성물 1

HCID 21890102HCID 21890102, 화합물수율 89%

시약·촉매·용매 2

HCID 962Water용매HCID 6212Chloroform용매

실험 절차

2-{4-[(6,7-Dimethoxy-4-quinolyl)oxy]phenoxy}acetic acid (150 mg), WSC.HCl (122 mg), and HOBT.H2O (86 mg) were dissolved in chloroform (5 ml) to prepare a solution. m-Anisidine (63 mg) was then added to the solution, and the mixture was heated under reflux for 3 hr. A saturated aqueous sodium hydrogencarbonate solution was added to the reaction solution, and the mixture was extracted with chloroform. The chloroform layer was washed with 1 N hydrochloric acid, water, and saturated brine and was then dried over anhydrous sodium sulfate. The solvent was removed by distillation under the reduced pressure. The residue was purified by thin-layer chromatography using chloroform/methanol for development to give the title compound (173 mg, yield 89%).

후처리

  1. customto prepare a solution
  2. temperaturethe mixture was heated
  3. temperatureunder reflux for 3 hr
  4. extractionthe mixture was extracted with chloroform
  5. washThe chloroform layer was washed with 1 N hydrochloric acid, water, and saturated brine
  6. dry with materialwas then dried over anhydrous sodium sulfate
  7. customThe solvent was removed by distillation under the reduced pressure
  8. customThe residue was purified by thin-layer chromatography

출처 및 근거

ORD 기록
ord-9ae5a64581084256a9d4e64ae5d134ab
출처 데이터셋
uspto-grants-2006_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07135466B2

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