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

HRID 460533

反応式

HRID 460533 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-171167bcfd7441389006929094d04ae9
出典データセット
uspto-grants-2007_03
特許番号
US07196202B2

関連ノート

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