Ethanol → HCID 68771264, 화합물

HRID 1170947

반응식

HRID 1170947 반응식
[OH:1][C:2]1[CH:3]=[CH:4][C:5]2[C:6](=[O:17])[C:7]3[C:12]([O:13][C:14]=2[CH:15]=1)=[CH:11][C:10]([OH:16])=[CH:9][CH:8]=3.C(O)C.[OH-].[K+].[C:23]([CH2:27][CH2:28][CH2:29][CH2:30][CH2:31]Br)([F:26])([F:25])[F:24]>O>[F:24][C:23]([F:26])([F:25])[CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][O:1][C:2]1[CH:3]=[CH:4][C:5]2[C:6](=[O:17])[C:7]3[C:12]([O:13][C:14]=2[CH:15]=1)=[CH:11][C:10]([OH:16])=[CH:9][CH:8]=3

참가 물질

6

반응물 4

HCID 702EthanolHCID 14797Potassium Hydroxide2회HCID 57493223,6-dihydroxy-9H-xanthen-9-oneHCID 138454716-Bromo-1,1,1-trifluorohexane

생성물 1

HCID 68771264HCID 68771264, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To 3,6-dihydroxy-xanthone (0.58 g, 1 equivalent) is added 10 ml of ethanol, then 117 mg of KOH 0.8 equivalents), followed by 0.58 g of CF3(CH2)5Br (1 equivalent); after two hours of boiling this mixture, the pH had dropped to the acidic range, and another 100 mg of KOH was added and heating continued overnight. The cooled mixture was diluted with water (50 ml) and extracted with ethyl acetate (3×50 ml), the combined extracts washed with 5 ml of water and brought to dryness. Separation of the 3-component mixture was achieved by chromatography (100 g of silica gel, column diameter 5 cm) with solvents of increasing polarity: Solvents used: ethyl acetate (A), hexane (isomeric mixture) (B), ethanol (C)

후처리

  1. additionthe pH had dropped to the acidic range
  2. temperatureheating continued overnight
  3. extractionextracted with ethyl acetate (3×50 ml)
  4. washthe combined extracts washed with 5 ml of water
  5. customSeparation of the 3-component mixture
  6. temperatureof increasing polarity

출처 및 근거

ORD 기록
ord-632095f8161a4f4bb137138c227a7b63
출처 데이터셋
uspto-grants-2010_11
특허 번호
US07829578B1

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