Water → HCID 22759220、化合物

HRID 329293ノート

反応式

HRID 329293 の反応式
[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]

参加物

7

反応物 4

HCID 962WaterHCID 73763-(Trifluoromethyl)phenolHCID 5360545SodiumHCID 22759269HCID 22759269、化合物

生成物 1

HCID 22759220HCID 22759220、化合物

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 3283Diethyl Ether溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-dabab43cac7649928b8a426b7c239a23
出典データセット
uspto-grants-1977_04
特許番号
US04020177

反応ノート

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