Dimethylformamide → HCID 69130305, 화합물

HRID 264356

반응식

HRID 264356 반응식
CN(C=O)C.[OH:6][C:7]1[CH:16]=[C:15]([OH:17])[CH:14]=[CH:13][C:8]=1[C:9]([O:11][CH3:12])=[O:10].C(=O)([O-])[O-].[K+].[K+].[CH2:24](Br)/[CH:25]=[C:26](/[CH2:28][CH2:29][CH:30]=[C:31]([CH3:33])[CH3:32])\[CH3:27]>O>[CH3:27]/[C:26](/[CH2:28][CH2:29][CH:30]=[C:31]([CH3:33])[CH3:32])=[CH:25]\[CH2:24][O:17][C:15]1[CH:14]=[CH:13][C:8]([C:9]([O:11][CH3:12])=[O:10])=[C:7]([OH:6])[CH:16]=1

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 11430Potassium CarbonateHCID 16523Methyl 2,4-DihydroxybenzoateHCID 53658672,6-Octadiene, 1-bromo-3,7-dimethyl-, (2E)-

생성물 1

HCID 69130305HCID 69130305, 화합물수율 76.2%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

In 80 m of DMF were poured 13.1 g (78.0 mmol) of methyl 2,4-dihydroxybenzoate and 18.9 g (86.9 mmol) of potassium carbonate, and 12.0 g (86.9 mmol) of geranyl bromide was added thereto dropwise at 5° C. After the addition, the mixture was stirred at room temperature for 1 hour, poured into 300 ml of water, and extracted with 250 ml of ethyl acetate. The extract was washed with water and a saturated sodium chloride aqueous solution, dried over sodium sulfate, and concentrated. The resulting crude product was purified by column chromatography to obtain 18.1 g (yield: 75%) of methyl 4-{(2E)-3,7-dimethylocta-2,6-dienyloxy}-2-hydroxybenzoate represented by the following chemical formula (hereinafter referred to as compound 31) as a colorless, clear and oily substance. The analytical results are shown below. ##STR52##

후처리

  1. additionwas added
  2. customdropwise at 5° C
  3. additionAfter the addition
  4. extractionextracted with 250 ml of ethyl acetate
  5. washThe extract was washed with water
  6. dry with materiala saturated sodium chloride aqueous solution, dried over sodium sulfate
  7. concentrationconcentrated
  8. customThe resulting crude product was purified by column chromatography

출처 및 근거

ORD 기록
ord-ed26f7e8ce11468380f41976500fe5b4
출처 데이터셋
uspto-grants-1997_07
특허 번호
US05646184

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