Hydrochloric Acid → HCID 178447998、化合物

HRID 54040

反応式

HRID 54040 の反応式
F[C:2]1[CH:7]=[CH:6][C:5](/[C:8](/[F:20])=[C:9](/[C@H:11]2[CH2:16][CH2:15][C@H:14]([CH2:17][CH2:18][CH3:19])[CH2:13][CH2:12]2)\[F:10])=[CH:4][CH:3]=1.Cl.[CH2:22]1[CH2:26]OC[CH2:23]1>>[CH2:23]([C@H:2]1[CH2:7][CH2:6][C@H:5](/[C:8](/[F:20])=[C:9](/[C@H:11]2[CH2:16][CH2:15][C@H:14]([CH2:17][CH2:18][CH3:19])[CH2:13][CH2:12]2)\[F:10])[CH2:4][CH2:3]1)[CH2:22][CH3:26]

参加物

4

反応物 3

HCID 313Hydrochloric AcidHCID 8028TetrahydrofuranHCID 178447996HCID 178447996、化合物

生成物 1

HCID 178447998HCID 178447998、化合物収率 60%

反応条件

温度
-10 °C

実験手順

Then, a mixed solution containing 1.3 g (6.31 mmol) of 2-(trans-4-n-propylcyclohexyl)-1,1,2-trifluoroethylene obtained in Example 1 and 10 ml of dry THF, was dropwise added thereto at the same temperature over a period of 15 minutes. The mixture was reacted at the same temperature for one hour and then the temperature was raised to -10° C. Then, 100 ml of 1N hydrochloric acid was added thereto. The organic layer was separated. The aqueous layer was extracted with n-hexane, and the extract was combined with the organic layer. The combined organic layer was washed with water and dried. Then, the solvent was distilled off, and the obtained crude solution was purified by silica gel column chromatography. The obtained solid was further recrystallized from ethanol to obtain 1.18 g (yield: 60%) of (E)-1,2-bis(trans-4-n-propylcyclohexyl)-1,2-difluoroethylene.

後処理

  1. additionwas dropwise added
  2. customThe mixture was reacted at the same temperature for one hour
  3. customThe organic layer was separated
  4. extractionThe aqueous layer was extracted with n-hexane
  5. washThe combined organic layer was washed with water
  6. customdried
  7. distillationThen, the solvent was distilled off
  8. customthe obtained crude solution
  9. customwas purified by silica gel column chromatography
  10. customThe obtained solid was further recrystallized from ethanol

出典と根拠

ORDレコード
ord-1564235662c9419a825d50edec702130
出典データセット
uspto-grants-1997_04
特許番号
US05621147

関連ノート

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