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Ethanol → 5'-Isopropyl-2'-methoxy-4-(trifluoromethyl)biphenyl-2-carbonitrile

HRID 217491
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HRID 217491 반응식
I[C:2]1[CH:9]=[CH:8][C:7]([C:10]([F:13])([F:12])[F:11])=[CH:6][C:3]=1[C:4]#[N:5].[CH:14]([C:17]1[CH:18]=[CH:19][C:20]([O:26][CH3:27])=[C:21](B(O)O)[CH:22]=1)([CH3:16])[CH3:15].C([O-])([O-])=O.[Na+].[Na+].C(O)C>CC(O)C(O)C.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.O>[CH:14]([C:17]1[CH:18]=[CH:19][C:20]([O:26][CH3:27])=[C:21]([C:2]2[C:3]([C:4]#[N:5])=[CH:6][C:7]([C:10]([F:13])([F:12])[F:11])=[CH:8][CH:9]=2)[CH:22]=1)([CH3:16])[CH3:15]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 702EthanolHCID 10340Sodium CarbonateHCID 45891905-Isopropyl-2-methoxyphenylboronic acidHCID 533636442-Iodo-5-(trifluoromethyl)benzonitrile

생성물 1

HCID 533636455'-Isopropyl-2'-methoxy-4-(trifluoromethyl)biphenyl-2-carbonitrile

시약·촉매·용매 3

HCID 178418397
HCID 178418397, 화합물
촉매
HCID 2622,3-Butanediol용매
HCID 962Water용매

실험 절차

To a solution of 2-iodo-5-(trifluoromethyl)benzonitrile (2.0 g, 6.7 mmol) and (5-isopropyl-2-methoxyphenyl)boronic acid (1.6 g, 8.4 mmol) in dimethyl ethylene glycol (30.4 mL) was added 2M Na2CO3 (6.8 mL), ethanol (9.6 mL), and water (10 mL). The solution was degassed with nitrogen for 2 minutes. Pd(PPh3)4 (774 mg, 0.67 mmol) was added and the solution was degassed with nitrogen again for 2 minutes. The solution was divided equally into two 40 mL microwave tubes. Each tube was degassed with nitrogen for 1 minute, sealed, and placed in a microwave reactor. The wattage was set for 200 W until the temperature reached 150° C. and then the temperature was held at 150° C. for ten minutes. The tubes were then cooled to room temperature, combined, poured into H2O (50 mL), and extracted with EtOAc (100 mL). The organic layer was washed with brine (50 mL), dried over Na2SO4, filtered, and concentrated. Purification by flash chromatography with 15% CH2Cl2/hexanes afforded 5′-isopropyl-2′-methoxy-4-(trifluoromethyl)biphenyl-2-carbonitrile as a light yellow oil. Rf=0.65 (25% EtOAc/hexanes). 1H NMR (CDCl3, 500 MHz) δ 7.97 (s, 1H), 7.85 (d, J=8.0 Hz, 1H), 7.63 (d, J=8.0 Hz, 1H), 7.31 (dd, J=8.5, 2.0 Hz, 1H), 7.12 (d, J=2.0 Hz, 1H), 6.97 (d, J=8.5 Hz, 1H), 3.82 (s, 3H), 2.93 (m, 1H), 1.27 (d, J=7.0 Hz, 6H).

후처리

  1. customThe solution was degassed with nitrogen for 2 minutes
  2. customthe solution was degassed with nitrogen again for 2 minutes
  3. customEach tube was degassed with nitrogen for 1 minute
  4. customsealed
  5. customplaced in a microwave reactor
  6. customreached 150° C.
  7. waitthe temperature was held at 150° C. for ten minutes
  8. additionpoured into H2O (50 mL)
  9. extractionextracted with EtOAc (100 mL)
  10. washThe organic layer was washed with brine (50 mL)
  11. dry with materialdried over Na2SO4
  12. filtrationfiltered
  13. concentrationconcentrated
  14. customPurification by flash chromatography with 15% CH2Cl2/hexanes

출처 및 근거

ORD 기록
ord-bcdcbedc1d594824b7a0c2ff19bdbba9
출처 데이터셋
uspto-grants-2012_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08193365B2

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