Water → 4-Hexyl-3-[(4-methoxycarbonylphenyl)methyl]aminobenzoic acid morpholide

HRID 2734

反応式

HRID 2734 の反応式
[NH2:1][C:2]1[CH:3]=[C:4]([CH:13]=[CH:14][C:15]=1[CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH3:21])[C:5]([N:7]1[CH2:12][CH2:11][O:10][CH2:9][CH2:8]1)=[O:6].[CH3:22][O:23][C:24]([C:26]1[CH:33]=[CH:32][C:29]([CH:30]=O)=[CH:28][CH:27]=1)=[O:25].O>C(O)(=O)C>[CH2:16]([C:15]1[CH:14]=[CH:13][C:4]([C:5]([N:7]2[CH2:8][CH2:9][O:10][CH2:11][CH2:12]2)=[O:6])=[CH:3][C:2]=1[NH:1][CH2:30][C:29]1[CH:28]=[CH:27][C:26]([C:24]([O:23][CH3:22])=[O:25])=[CH:33][CH:32]=1)[CH2:17][CH2:18][CH2:19][CH2:20][CH3:21]

参加物

5

反応物 3

HCID 962WaterHCID 15294Methyl 4-FormylbenzoateHCID 539494553-Amino-4-hexylbenzoic acid morpholide

生成物 1

HCID 867517094-Hexyl-3-[(4-methoxycarbonylphenyl)methyl]aminobenzoic acid morpholide

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

The compound ([5]-(55)-75) (600 mg) prepared in Example 63 was dissolved in acetic acid (6.0 ml). Then, 4-methoxycarbonylbenzaldehyde (373 mg) was added. The mixture was stirred at room temperature for 4 hours. Then, boranediethylamine complex (146 mg) was added to the solution. The mixture was stirred at room temperature for 30 minutes. After the reaction was completed, water was added to the solution. The solution was extracted with ethyl acetate, washed with distilled water, and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (Kieselgel 60=30 g, hexane/ethyl acetate=1/1) to obtain the above-captioned compound ([5]-(57)-75') (841 mg) as a white solid.

後処理

  1. stirringThe mixture was stirred at room temperature for 30 minutes
  2. extractionThe solution was extracted with ethyl acetate
  3. washwashed with distilled water
  4. dry with materialdried over anhydrous sodium sulfate
  5. customThe solvent was evaporated under reduced pressure
  6. customthe residue was purified by silica gel column chromatography (Kieselgel 60=30 g, hexane/ethyl acetate=1/1)
  7. customto obtain the above-captioned compound ([5]-(57)-75') (841 mg) as a white solid

出典と根拠

ORDレコード
ord-20fb073b44614d5f8991584cce60fb11
出典データセット
uspto-grants-1998_03
特許番号
US05731310

関連ノート

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