Water → HCID 69130364, 화합물

HRID 264361노트

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HRID 264361 반응식
[NH2:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[C:4]([OH:11])[CH:3]=1.[CH2:12](Br)/[CH:13]=[C:14](/[CH2:16][CH2:17][CH:18]=[C:19]([CH3:21])[CH3:20])\[CH3:15].O>CN(C=O)C>[CH3:15]/[C:14](/[CH2:16][CH2:17][CH:18]=[C:19]([CH3:21])[CH3:20])=[CH:13]\[CH2:12][NH:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[C:4]([OH:11])[CH:3]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 46494-Aminosalicylic AcidHCID 53658672,6-Octadiene, 1-bromo-3,7-dimethyl-, (2E)-

생성물 1

HCID 69130364HCID 69130364, 화합물수율 7.6%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

In 30 ml of DMF was dissolved 2.12 g (13.8 mmol) of 4-amino-2-hydroxybenzoic acid, and 3.0 g (13.8 mmol) of geranyl bromide was added thereto. After the mixture was stirred at room temperature for 4 hours, water was added thereto, and the mixture was extracted with ethyl acetate. The organic layer was washed with water and a saturated sodium chloride aqueous solution, dried over anhydrous sodium sulfate, and concentrated. The resulting crude product was purified by column chromatography and recrystallized from ethyl acetate/hexane to obtain 0.30 g (yield: 7.6%) of N-{(2E)-3,7-dimethylocta-2,6-dienyl}-4-amino-2-hydroxybenzoic acid represented by the following structural formula (hereinafter referred to as compound 47) as white crystals. The analytical results are shown below. ##STR68##

후처리

  1. additionwas added
  2. extractionthe mixture was extracted with ethyl acetate
  3. washThe organic layer was washed with water
  4. dry with materiala saturated sodium chloride aqueous solution, dried over anhydrous sodium sulfate
  5. concentrationconcentrated
  6. customThe resulting crude product was purified by column chromatography
  7. customrecrystallized from ethyl acetate/hexane

출처 및 근거

ORD 기록
ord-5316f008abab4fd7b2c48ac561965c04
출처 데이터셋
uspto-grants-1997_07
특허 번호
US05646184

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