Water → HCID 69130364、化合物

HRID 264361

反応式

HRID 264361 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 69130364HCID 69130364、化合物収率 7.6%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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##

後処理

  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

出典と根拠

ORDレコード
ord-5316f008abab4fd7b2c48ac561965c04
出典データセット
uspto-grants-1997_07
特許番号
US05646184

関連ノート

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