Water → 3-(5-Tert-butyl-2-phenyl-4,5,6,7-tetrahydroindol-1-yl)benzoic acid

HRID 2244304ノート

反応式

HRID 2244304 の反応式
[C:1]([CH:5]1[CH2:10][CH2:9][C:8](=O)[CH:7]([CH2:12][C:13](=O)[C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[CH2:6]1)([CH3:4])([CH3:3])[CH3:2].[NH2:21][C:22]1[CH:23]=[C:24]([CH:28]=[CH:29][CH:30]=1)[C:25]([OH:27])=[O:26].O>C(O)(=O)C>[C:1]([CH:5]1[CH2:10][CH2:9][C:8]2[N:21]([C:22]3[CH:23]=[C:24]([CH:28]=[CH:29][CH:30]=3)[C:25]([OH:27])=[O:26])[C:13]([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)=[CH:12][C:7]=2[CH2:6]1)([CH3:4])([CH3:3])[CH3:2]

参加物

5

反応物 3

HCID 962WaterHCID 74193-Aminobenzoic AcidHCID 122703414-Tert-butyl-2-(2-oxo-2-phenylethyl)-cyclohexanone

生成物 1

HCID 116031913-(5-Tert-butyl-2-phenyl-4,5,6,7-tetrahydroindol-1-yl)benzoic acid収率 41%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A solution of 4-tert-butyl-2-(2-oxo-2-phenylethyl)-cyclohexanone (0.219 gm) in glacial acetic acid (3.0 mL) in a 25-mL round-bottomed flask, under nitrogen, was fitted with a heating mantle and reflux condenser. To this solution was added 3-aminobenzoic acid (0.138 gm), which was then heated at 110 C for 3 hr. The solution was cooled to ambient temperature, 8 mL water was added, and the suspension was stirred 18 hr under nitrogen. The solid was filtered, washed with water, and recrystallized in acetonitrile to provide 0.123 gm of the pure product.

後処理

  1. temperaturereflux condenser
  2. temperaturewas then heated at 110 C for 3 hr
  3. filtrationThe solid was filtered
  4. washwashed with water
  5. customrecrystallized in acetonitrile

出典と根拠

ORDレコード
ord-98121952e784467fa6d7c23e4b6d252c
出典データセット
uspto-grants-2010_03
特許番号
US07678823B2

反応ノート

読み込み中…