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Methyl 6-formylpyridine-3-carboxylate → Methyl 6-(1-(2,6-dimethyl-4'-(trifluoromethyl)biphenyl-4-ylamino)-3-methylbutyl)nicotinate

HRID 2173799
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HRID 2173799 반응식
[CH:1]([C:3]1[CH:12]=[CH:11][C:6]([C:7]([O:9][CH3:10])=[O:8])=[CH:5][N:4]=1)=O.[CH3:13][C:14]1[CH:19]=[C:18]([NH2:20])[CH:17]=[C:16]([CH3:21])[C:15]=1[C:22]1[CH:27]=[CH:26][C:25]([C:28]([F:31])([F:30])[F:29])=[CH:24][CH:23]=1>C1(C)C=CC=CC=1>[CH3:13][C:14]1[CH:19]=[C:18]([NH:20][CH:1]([C:3]2[CH:12]=[CH:11][C:6]([C:7]([O:9][CH3:10])=[O:8])=[CH:5][N:4]=2)[CH2:5][CH:6]([CH3:11])[CH3:7])[CH:17]=[C:16]([CH3:21])[C:15]=1[C:22]1[CH:27]=[CH:26][C:25]([C:28]([F:30])([F:29])[F:31])=[CH:24][CH:23]=1
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HCID 586269Methyl 6-formylpyridine-3-carboxylateHCID 674849042,6-Dimethyl-4'-(trifluoromethyl)biphenyl-4-amine

생성물 1

HCID 67980659Methyl 6-(1-(2,6-dimethyl-4'-(trifluoromethyl)biphenyl-4-ylamino)-3-methylbutyl)nicotinate수율 101.9%

시약·촉매·용매 1

HCID 1140Toluene용매

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온도
90 °C

실험 절차

To a solution of methyl 6-formylnicotinate (200 mg, 1.21 mmol) in toluene (8 mL) containing activated molecular sieves was added 2,6-dimethyl-4′-(trifluoromethyl)biphenyl-4-amine (316 mg, 1.33 mmol). The reaction mixture was heated to 90° C. and stirred overnight. The reaction mixture was concentrated and the residue dissolved in tetrahydrofuran (8 mL). The solution was cooled to 0° C. Zinc chloride (3.64 mL of a 1.0M solution in diethyl ether, 3.64 mmol) was added, followed by isobutylmagnesium bromide (1.82 mL of a 2.0M solution in THF, 3.64 mmol). The reaction mixture was stirred at 0° C. for 2 h. The reaction was quenched with saturated aqueous ammonium chloride (5 mL). The mixture was diluted with dichloromethane (30 mL) and water (30 mL). The layers were separated and the aqueous layer was extracted with dichloromethane (30 mL) two more times. The combined organic layers were dried over sodium sulfate, filtered, and concentrated. Purification by column chromatography gave methyl 6-(1-(2,6-dimethyl-4′-(trifluoromethyl)biphenyl-4-ylamino)-3-methylbutyl)nicotinate (290 mg, 51%). 1H NMR (400 MHz, CDCl3, δ): 9.20 (s, 1H), 8.25 (d, 1H), 7.62 (d, 4H), 7.50 (d, 2H), 7.45 (d, 1H), 7.20 (d, 2H), 6.30 (s, 2H), 4.62 (m, 1H), 3.95 (s, 3H), 3.5 (s, 3H), 1.87 (s, 6H), 1.73 (d, 3H), 1.26 (m, 3H), 1.10 (m, 6H).

후처리

  1. concentrationThe reaction mixture was concentrated
  2. dissolutionthe residue dissolved in tetrahydrofuran (8 mL)
  3. temperatureThe solution was cooled to 0° C
  4. additionZinc chloride (3.64 mL of a 1.0M solution in diethyl ether, 3.64 mmol) was added
  5. stirringThe reaction mixture was stirred at 0° C. for 2 h
  6. customThe reaction was quenched with saturated aqueous ammonium chloride (5 mL)
  7. additionThe mixture was diluted with dichloromethane (30 mL) and water (30 mL)
  8. customThe layers were separated
  9. extractionthe aqueous layer was extracted with dichloromethane (30 mL) two more times
  10. dry with materialThe combined organic layers were dried over sodium sulfate
  11. filtrationfiltered
  12. concentrationconcentrated
  13. customPurification by column chromatography

출처 및 근거

ORD 기록
ord-c6949f5561fd468cb44f4a00c3bafcae
출처 데이터셋
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09056834B2

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