홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

4'-Hydroxy-4-biphenylcarbonitrile → 4-(3-Hydroxy-propoxy)-benzoic acid 4'-cyanobiphenyl-4-yl ester

HRID 890901
노트
인쇄 미리보기

반응식

HRID 890901 반응식
[Si]([O:8][CH2:9][CH2:10][CH2:11][O:12][C:13]1[CH:21]=[CH:20][C:16]([C:17]([OH:19])=[O:18])=[CH:15][CH:14]=1)(C(C)(C)C)(C)C.O[C:23]1[CH:28]=[CH:27][C:26]([C:29]2[CH:34]=[CH:33][C:32]([C:35]#[N:36])=[CH:31][CH:30]=2)=[CH:25][CH:24]=1>C(Cl)Cl>[C:35]([C:32]1[CH:33]=[CH:34][C:29]([C:26]2[CH:25]=[CH:24][C:23]([O:19][C:17](=[O:18])[C:16]3[CH:15]=[CH:14][C:13]([O:12][CH2:11][CH2:10][CH2:9][OH:8])=[CH:21][CH:20]=3)=[CH:28][CH:27]=2)=[CH:30][CH:31]=1)#[N:36]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 1406104'-Hydroxy-4-biphenylcarbonitrileHCID 222424964-(3-{[tert-Butyl(dimethyl)silyl]oxy}propoxy)benzoic acid

생성물 1

HCID 235977644-(3-Hydroxy-propoxy)-benzoic acid 4'-cyanobiphenyl-4-yl ester수율 89%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
40 °C

실험 절차

To a solution of 2 (10 g, 32.21 mmol), 4′-hydroxy-biphenyl-4-carbonitrile (6.35 g, 32.53 mmol), and toluenesulfonic/4-(dimethylamino)pyridine complex (0.95 g, 3.22 mmol) in anhydrous methylene chloride (100 mL) was added N,N-dicyclohexylcarbodiimide (6.98 g, 33.82 mmol) under argon. The reaction mixture was stirred at 40° C. overnight. Upon filtering off the white residues, the filtrate was diluted with additional methylene chloride. The solution was then washed with water. The silyl ether of the title compound was purified by flash column chromatography on silica gel with gradient elution from 0 to 2% acetone in methylene chloride. The silyl-protected compound was hydrolyzed in tetrahydrofuran: water:acetic acid (80 mL: 80 mL: 240 mL) overnight. The volume of the solution was reduced by 50% via evaporation under reduced pressure. Methylene chloride was added to the slurry for washing sequentially with H2O, a 10% NaHCO3 solution and brine before drying over anhydrous MgSO4. The crude product resulting from evaporation of the solvent was purified by recrystallization from ethanol to yield 3 (10.71 g, 89%). 1H NMR spectral data (400 MHz, CDCl3): δ 2.10 (quintet, 2H, —CH2—), δ 3.95 (t, 2H, —CH2OAr), δ 4.25 (t, 2H, HOCH2—), δ 7.00–8.25 (m, 12H, aromatic rings).

후처리

  1. filtrationUpon filtering off the white residues
  2. additionthe filtrate was diluted with additional methylene chloride
  3. washThe solution was then washed with water
  4. customThe silyl ether of the title compound was purified by flash column chromatography on silica gel with gradient elution from 0 to 2% acetone in methylene chloride
  5. customacetic acid (80 mL: 80 mL: 240 mL) overnight
  6. customThe volume of the solution was reduced by 50% via evaporation under reduced pressure
  7. additionMethylene chloride was added to the slurry
  8. washfor washing sequentially with H2O
  9. dry with materiala 10% NaHCO3 solution and brine before drying over anhydrous MgSO4
  10. customThe crude product resulting from evaporation of the solvent
  11. customwas purified by recrystallization from ethanol

출처 및 근거

ORD 기록
ord-b13dda1bfc7e4c2aa09ea5f393f5a97a
출처 데이터셋
uspto-grants-2006_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07001648B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트