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

HRID 460532

反応式

HRID 460532 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.[CH3:25][O:26][C:27](OC)(OC)OC.[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:25]([O:26][CH3:27])[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 74613Tetramethyl orthocarbonateHCID 120430856-(3-Phenylamino-4-aminophenyl)oxyhexanoic acid methyl ester

生成物 1

HCID 99692876-[[2-Methoxy-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 0.12 ml of tetramethylorthocarbonate 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. 104 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. custom104 mg was obtained

出典と根拠

ORDレコード
ord-cc4cad887e00467faafc24f3bc557a5f
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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