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Water → HCID 178448098, 화합물

HRID 1194638
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HRID 1194638 반응식
[F:1][C:2]1[CH:3]=[C:4]([C:9]2[CH:14]=[CH:13][C:12]([OH:15])=[CH:11][CH:10]=2)[CH:5]=[CH:6][C:7]=1[F:8].[CH2:16]([C@H:19]1[CH2:24][CH2:23][C@H:22]([C:25](Cl)=[O:26])[CH2:21][CH2:20]1)[CH2:17][CH3:18].O>N1C=CC=CC=1.C1(C)C=CC=CC=1>[CH2:16]([C@H:19]1[CH2:24][CH2:23][C@H:22]([C:25]([O:15][C:12]2[CH:13]=[CH:14][C:9]([C:4]3[CH:5]=[CH:6][C:7]([F:8])=[C:2]([F:1])[CH:3]=3)=[CH:10][CH:11]=2)=[O:26])[CH2:21][CH2:20]1)[CH2:17][CH3:18]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 962WaterHCID 113677374-(3,4-Difluorophenyl)phenolHCID 178448094HCID 178448094, 화합물

생성물 1

HCID 178448098HCID 178448098, 화합물수율 70%

시약·촉매·용매 2

HCID 1049Pyridine용매HCID 1140Toluene용매

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온도
60 °C

실험 절차

3,4-Difluoro-4'-hydroxybiphenyl (2.0 g, 10 mmols) was dissolved in dried pyridine (5 cc), followed by adding to the solution, a solution obtained by dissolving trans-4-propylcyclohexanecarboxylic acid chloride (2 g, 11 mmols) in dry toluene (10 cc), heating the mixture at 60° C. for 3 hours with stirring, then adding the resulting material to water (100 cc), then washing the separated toluene layer with 6N hydrochloric acid, 2N aqueous solution of NaOH and further with water, distilling off toluene from the toluene layer, and recrystallizing the residual crystals from ethyl acetate (10 cc) to obtain the objective 3,4-difluoro-4'-biphenylyl trans-4-propylcyclohexanecarboxylate (2.5 g, 70%).

후처리

  1. additionby adding to the solution
  2. customa solution obtained
  3. washwashing the separated toluene layer with 6N hydrochloric acid, 2N aqueous solution of NaOH
  4. distillationfurther with water, distilling off toluene from the toluene layer
  5. customrecrystallizing the residual crystals from ethyl acetate (10 cc)

출처 및 근거

ORD 기록
ord-06d39788c1ff494891dfe5e1cc1c27de
출처 데이터셋
uspto-grants-1989_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04816179

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