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

HRID 2120502노트

반응식

HRID 2120502 반응식
[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

참가 물질

4

반응물 1

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

생성물 1

HCID 178466566HCID 178466566, 화합물수율 100%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 21863594Toluene ethanol용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-999d441aa631417fb021d908d1812ea9
출처 데이터셋
uspto-grants-2004_02
특허 번호
US06692657B1

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