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

HRID 1504995노트

반응식

HRID 1504995 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-05642a40eefd482190fa46fe6b06715b
출처 데이터셋
uspto-grants-2015_12
특허 번호
US09216966B2

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