Triethylsilane → 4-Bromo-2-fluoro-4'-propyl-1,1'-biphenyl

HRID 1755615

반응식

HRID 1755615 반응식
[F:1][C:2]1[CH:7]=[C:6]([Br:8])[CH:5]=[CH:4][C:3]=1[C:9]1[CH:14]=[CH:13][C:12]([C:15](=O)[CH2:16][CH3:17])=[CH:11][CH:10]=1.C([SiH](CC)CC)C.C(=O)([O-])O.[Na+]>FC(F)(F)C(O)=O>[F:1][C:2]1[CH:7]=[C:6]([Br:8])[CH:5]=[CH:4][C:3]=1[C:9]1[CH:14]=[CH:13][C:12]([CH2:15][CH2:16][CH3:17])=[CH:11][CH:10]=1

참가 물질

5

반응물 3

HCID 12052TriethylsilaneHCID 516892Sodium BicarbonateHCID 8220021-(4'-Bromo-2'-fluorobiphenyl-4-yl)propan-1-one

생성물 1

HCID 227175064-Bromo-2-fluoro-4'-propyl-1,1'-biphenyl수율 84.5%

시약·촉매·용매 1

HCID 6422Trifluoroacetic acid용매2회

실험 절차

29 g of 2-fluoro-4-bromo-4'-propionylbiphenyl was dissolved in 72 ml of trifluoroacetic acid and stirred. 24 g of triethylsilane was dropwise added thereto at room temperature over a period of 30 minutes. After this was stirred for 2 hours, 900 ml of an aqueous saturated sodium hydrogencarbonate solution was dropwise added thereto so that the excess trifluoroacetic acid was decomposed. This was extracted with chloroform and then washed three times with water, and chloroform was removed by distillation. The residue was distilled under reduced pressure (b.p. 140° to 145° C./2 mmHg) to obtain 23.4 g of 2-fluoro-4-bromo-4'-propylbiphenyl.

후처리

  1. stirringAfter this was stirred for 2 hours
  2. extractionThis was extracted with chloroform
  3. washwashed three times with water, and chloroform
  4. customwas removed by distillation
  5. distillationThe residue was distilled under reduced pressure (b.p. 140° to 145° C./2 mmHg)

출처 및 근거

ORD 기록
ord-3354ee80d5dd44989ab7c0622cfa8bf5
출처 데이터셋
uspto-grants-1995_08
특허 번호
US05437815

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