2-(2-(4-(2,3-Difluoro-4-ethoxyphenyl)cyclohexylidene)-ethyl)-1,3-dioxane → HCID 178466566、化合物

HRID 1793273ノート

反応式

HRID 1793273 の反応式
[F:1][C:2]1[C:7]([F:8])=[C:6]([O:9][CH2:10][CH3:11])[CH:5]=[CH:4][C:3]=1[CH:12]1[CH2:17][CH2:16][C:15](=[CH:18][CH2:19][CH:20]2[O:25][CH2:24][CH2:23][CH2:22][O:21]2)[CH2:14][CH2:13]1>C1(C)C=CC=CC=1.C(O)C.[Pd]>[F:1][C:2]1[C:7]([F:8])=[C:6]([O:9][CH2:10][CH3:11])[CH:5]=[CH:4][C:3]=1[C@H:12]1[CH2:13][CH2:14][C@H:15]([CH2:18][CH2:19][CH:20]2[O:21][CH2:22][CH2:23][CH2:24][O:25]2)[CH2:16][CH2:17]1

参加物

4

反応物 1

HCID 220205192-(2-(4-(2,3-Difluoro-4-ethoxyphenyl)cyclohexylidene)-ethyl)-1,3-dioxane

生成物 1

HCID 178466566HCID 178466566、化合物収率 100%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 21863594Toluene ethanol溶媒

実験手順

The 2-(2-(4-(2,3-difluoro-4-ethoxyphenyl)cyclohexylidene)-ethyl)-1,3-dioxane (36.9 mmol) obtained by the reaction of Step 3 was dissolved in 100 ml of a mixed solvent of toluene/ethanol (1/1), 4.0 g of 5-wt %-palladium/carbon catalyst was added, and the solution was stirred for 7 hours at room temperature under a hydrogen pressure of 1–2 kg/cm2. After the catalyst was filtered off, the solvent was distilled off from the filtrate under reduced pressure, the residue was subjected to silica gel column chromatography (eluent: a mixed solvent of ethyl acetate/toluene=3/7), the solvent was distilled off under reduced pressure, and the product was re-crystallized from ethanol to form 2-(2-(trans-4-(2,3-difluoro-4-ethoxyphenyl)-cyclohexyl)-ethyl)-1,3-dioxane (36.9 mmol).

後処理

  1. additionwas added
  2. filtrationAfter the catalyst was filtered off
  3. distillationthe solvent was distilled off from the filtrate under reduced pressure
  4. distillationa mixed solvent of ethyl acetate/toluene=3/7), the solvent was distilled off under reduced pressure
  5. customthe product was re-crystallized from ethanol

出典と根拠

ORDレコード
ord-ce76130bc77244d494327549fffb2ce1
出典データセット
uspto-grants-2006_07
特許番号
US07081279B2

反応ノート

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