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Bromine → 3'-Bromo-4'-(2-methylbutyloxy)-4-p-toluenesulfonylbiphenyl

HRID 648868
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HRID 648868 반응식
[CH3:1][CH:2]([CH2:27][CH3:28])[CH2:3][O:4][C:5]1[CH:10]=[CH:9][C:8]([C:11]2[CH:16]=[CH:15][C:14]([S:17]([C:20]3[CH:25]=[CH:24][C:23]([CH3:26])=[CH:22][CH:21]=3)(=[O:19])=[O:18])=[CH:13][CH:12]=2)=[CH:7][CH:6]=1.[Br:29]Br.S([O-])(O)=O.[Na+]>C(Cl)(Cl)(Cl)Cl>[Br:29][C:10]1[CH:9]=[C:8]([C:11]2[CH:16]=[CH:15][C:14]([S:17]([C:20]3[CH:21]=[CH:22][C:23]([CH3:26])=[CH:24][CH:25]=3)(=[O:19])=[O:18])=[CH:13][CH:12]=2)[CH:7]=[CH:6][C:5]=1[O:4][CH2:3][CH:2]([CH3:1])[CH2:27][CH3:28]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 24408Bromine2회HCID 20143995HCID 20143995, 화합물HCID 23665763Sodium Bisulfite

생성물 1

HCID 201440033'-Bromo-4'-(2-methylbutyloxy)-4-p-toluenesulfonylbiphenyl수율 113.2%

시약·촉매·용매 1

HCID 5943Carbon Tetrachloride용매2회

실험 절차

4'-(2-methylbutyloxy)-4-p-toluenesulfonylbiphenyl (41 g) prepared in the above step (ii) was dissolved in CCl4 (400 ml). To the resulting solution was dropwise added bromine (25 g) dissolved in CCl4 (100 ml), at room temperature over one hour, followed by stirring at room temperature for 5 hours, adding an aqueous solution of sodium hydrogen sulfite till the color of bromine disappeared, separating the organic layer, washing with 6N hydrochloric acid, washing with an aqueous solution of 2N NaOH, washing with water to make the solution neutral, drying and distilling off CCl4 to obtain oily 3'-bromo-4'-(2-methylbutyloxy)-4-p-toluenesulfonylbiphenyl (55.7 g).

후처리

  1. customseparating the organic layer
  2. washwashing with 6N hydrochloric acid
  3. washwashing with an aqueous solution of 2N NaOH
  4. washwashing with water
  5. customdrying
  6. distillationdistilling off CCl4

출처 및 근거

ORD 기록
ord-0bdd5c5951ed4243840eaf0e8229fe1c
출처 데이터셋
uspto-grants-1988_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04737313

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