Water → HCID 22759220, 화합물

HRID 460857노트

반응식

HRID 460857 반응식
[Na].[F:2][C:3]([F:12])([F:11])[C:4]1[CH:5]=[C:6]([OH:10])[CH:7]=[CH:8][CH:9]=1.[C:13]([CH:16]([CH2:28][CH2:29][CH2:30][CH:31]1[O:33][CH2:32]1)[CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][C:23]([O:25][CH2:26][CH3:27])=[O:24])(=[O:15])[CH3:14].O>C(O)C.CCOCC>[C:13]([CH:16]([CH2:28][CH2:29][CH2:30][CH:31]([OH:33])[CH2:32][O:10][C:6]1[CH:7]=[CH:8][CH:9]=[C:4]([C:3]([F:11])([F:12])[F:2])[CH:5]=1)[CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][C:23]([O:25][CH2:26][CH3:27])=[O:24])(=[O:15])[CH3:14]

참가 물질

7

반응물 4

HCID 962WaterHCID 73763-(Trifluoromethyl)phenolHCID 5360545SodiumHCID 22759269HCID 22759269, 화합물

생성물 1

HCID 22759220HCID 22759220, 화합물

시약·촉매·용매 2

HCID 702Ethanol용매HCID 3283Diethyl Ether용매

실험 절차

Sodium (1.15 g., 0.05 mole) is dissolved in ethanol (60 ml.). 3-Trifluoromethylphenol (14.6 g., 0.09 mole) is added and then ethyl 8-acetyl-12,13-epoxytridecanoate (13.0 g., 0.0435 mole). The resulting solution is heated under reflux for 1.5 hour. It is then cooled and poured into 300 ml. of water. The oily product is taken up in ether, washed with 100 ml. of 5% sodium hydroxide solution, water and brine and dried over sodium sulfate. The ether is evaporated in vacuo leaving 17.4 g. of the title compound as a yellow oil. It is used in the next step without purification.

후처리

  1. temperatureThe resulting solution is heated
  2. temperatureunder reflux for 1.5 hour
  3. temperatureIt is then cooled
  4. additionpoured into 300 ml
  5. washwashed with 100 ml
  6. dry with materialof 5% sodium hydroxide solution, water and brine and dried over sodium sulfate
  7. customThe ether is evaporated in vacuo
  8. customleaving 17.4 g

출처 및 근거

ORD 기록
ord-e667d5947a244450ad0d3127302f43e4
출처 데이터셋
uspto-grants-1977_12
특허 번호
US04061643

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