Sodium Hydroxide → 2-{4-[2-(3,4-Dichloro-phenyl)-ethyl]phenylamino}-5-nitrobenzoic acid

HRID 488485노트

반응식

HRID 488485 반응식
C[O:2][C:3](=[O:30])[C:4]1[CH:9]=[C:8]([N+:10]([O-:12])=[O:11])[CH:7]=[CH:6][C:5]=1[NH:13][C:14]1[CH:19]=[CH:18][C:17]([CH2:20][CH2:21][C:22]2[CH:27]=[CH:26][C:25]([Cl:28])=[C:24]([Cl:29])[CH:23]=2)=[CH:16][CH:15]=1.[OH-].[Na+]>CCO.C1COCC1>[Cl:29][C:24]1[CH:23]=[C:22]([CH2:21][CH2:20][C:17]2[CH:18]=[CH:19][C:14]([NH:13][C:5]3[CH:6]=[CH:7][C:8]([N+:10]([O-:12])=[O:11])=[CH:9][C:4]=3[C:3]([OH:30])=[O:2])=[CH:15][CH:16]=2)[CH:27]=[CH:26][C:25]=1[Cl:28]

참가 물질

5

반응물 2

HCID 14798Sodium HydroxideHCID 537377402-{4-[2-(3,4-Dichloro-phenyl)-ethyl]phenylamino}-5-nitrobenzoic acid methyl ester

생성물 1

HCID 99324612-{4-[2-(3,4-Dichloro-phenyl)-ethyl]phenylamino}-5-nitrobenzoic acid수율 100%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 8028Tetrahydrofuran용매

실험 절차

A solution of 2-{4-[2-(3,4-dichloro-phenyl)-ethyl]phenylamino}-5-nitrobenzoic acid methyl ester (340 mg, 0.76 mmol) and 1N NaOH (aq.) (4.0 mL) in EtOH (4.0 mL) and THF (4.0 mL) was heated to reflux for 16 hours. The solvent was removed in vacuum. The residue was diluted with H2O and acidified with concentrated HCl to pH 1. The mixture was then extracted with methylene chloride, dried (Na2SO4), filtered and concentrated in vacuo to yield a yellow solid, 329 mg (0.76 mmol, 100%) of the desired product mp 214-217° C.

후처리

  1. temperatureto reflux for 16 hours
  2. customThe solvent was removed in vacuum
  3. additionThe residue was diluted with H2O
  4. extractionThe mixture was then extracted with methylene chloride
  5. dry with materialdried (Na2SO4)
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-f1c676206daa482c8d1737adb93f695d
출처 데이터셋
uspto-grants-2005_12
특허 번호
US06972287B1

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