Sodium Hydroxide → 6-[[2-Ethoxy-1-phenyl-1H-benzimidazol-6-yl]oxy]Hexanoic Acid Methyl Ester

HRID 460533

반응식

HRID 460533 반응식
[CH3:1][O:2][C:3](=[O:24])[CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][O:9][C:10]1[CH:15]=[CH:14][C:13]([NH2:16])=[C:12]([NH:17][C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[CH:11]=1.[CH2:25]([O:27][C:28](OCC)(OCC)OCC)[CH3:26].[OH-].[Na+]>C(O)(=O)C>[CH3:1][O:2][C:3](=[O:24])[CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][O:9][C:10]1[CH:15]=[CH:14][C:13]2[N:16]=[C:28]([O:27][CH2:25][CH3:26])[N:17]([C:18]3[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=3)[C:12]=2[CH:11]=1

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 66213Tetraethyl orthocarbonateHCID 120430856-(3-Phenylamino-4-aminophenyl)oxyhexanoic acid methyl ester

생성물 1

HCID 102214996-[[2-Ethoxy-1-phenyl-1H-benzimidazol-6-yl]oxy]Hexanoic Acid Methyl Ester

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

200 mg of 6-(3-phenylamino-4-aminophenyl)oxyhexanoic acid methyl ester was mixed with 0.19 ml of tetraethylorthocarbonate and 40 μl of acetic acid, and the mixture was heated for 4 hours to 80° C. After cooling, it was mixed with 1N sodium hydroxide solution, extracted three times with ethyl acetate, the combined organic phases were washed with saturated sodium chloride solution, dried on sodium sulfate and concentrated by evaporation in a vacuum. The residue was purified by column chromatography on silica gel. 124 mg was obtained.

후처리

  1. temperaturethe mixture was heated for 4 hours to 80° C
  2. temperatureAfter cooling
  3. extractionextracted three times with ethyl acetate
  4. washthe combined organic phases were washed with saturated sodium chloride solution
  5. customdried on sodium sulfate
  6. concentrationconcentrated by evaporation in a vacuum
  7. customThe residue was purified by column chromatography on silica gel
  8. custom124 mg was obtained

출처 및 근거

ORD 기록
ord-171167bcfd7441389006929094d04ae9
출처 데이터셋
uspto-grants-2007_03
특허 번호
US07196202B2

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