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Methyl 6-formylpyridine-3-carboxylate → HCID 67980582, 화합물

HRID 1427453
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HRID 1427453 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.[F:13][C:14]([F:29])([F:28])[C:15]1[CH:20]=[CH:19][C:18]([C:21]2[CH:26]=[CH:25][C:24]([NH2:27])=[CH:23][CH:22]=2)=[CH:17][CH:16]=1.[CH2:30]([Mg]Br)[CH:31]([CH3:33])[CH3:32]>O1CCCC1.[Cl-].[Zn+2].[Cl-]>[CH3:30][CH:31]([CH3:33])[CH2:32][CH:1]([C:3]1[CH:12]=[CH:11][C:6]([C:7]([O:9][CH3:10])=[O:8])=[CH:5][N:4]=1)[NH:27][C:24]1[CH:25]=[CH:26][C:21]([C:18]2[CH:19]=[CH:20][C:15]([C:14]([F:28])([F:29])[F:13])=[CH:16][CH:17]=2)=[CH:22][CH:23]=1
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참가 물질

6

반응물 3

HCID 586269Methyl 6-formylpyridine-3-carboxylateHCID 27827094'-(Trifluoromethyl)[1,1'-biphenyl]-4-amineHCID 178418816HCID 178418816, 화합물

생성물 1

HCID 67980582HCID 67980582, 화합물수율 39.2%

시약·촉매·용매 2

HCID 3007855Zincchloride촉매
HCID 8028
Tetrahydrofuran
용매

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온도
90 °C

실험 절차

To a solution of methyl 6-formylnicotinate (0.200 g, 1.21 mmol) in tetrahydrofuran (8 mL) containing activated molecular sieves was added 4′-(trifluoromethyl)biphenyl-4-amine (316 mg, 1.33 mmol). The reaction was heated to 90° C. and stirred overnight. The reaction was concentrated to dryness and the residue was dissolved in tetrahydrofuran (8 mL). The solution was cooled to 0° C. Zinc chloride (3.52 mL, 1M in diethyl ether, 3.52 mmol) was added, followed by isobutylmagnesium bromide (1.47 mL, 2.0M in THF, 3.52 mmol). The reaction was stirred at 0° C. for 2 hours. The reaction was quenched with saturated ammonium chloride. The mixture was diluted with dichloromethane and water. The layers were separated and the aqueous was extracted again with dichloromethane. The combined organic layers were dried over sodium sulfate, filtered and concentrated. Purification by column chromatography gave methyl 6-(3-methyl-1-(4′-(trifluoromethyl)biphenyl-4-ylamino)butyl)nicotinate (210 mg, 39%) as a yellow oil. 1H NMR (400 MHz, CD3OD, δ): 9.09 (s, 1H), 8.31 (d, 1H), 7.72-7.57 (m, 5H), 7.41 (d, 2H), 6.65 (d, 2H), 4.61-4.52 (m, 1H), 3.94 (s, 3H), 1.92-1.73 (m, 2H), 1.1.72-1.61 (m, 1H), 1.05 (d, 3H), 0.91 (d, 3H).

후처리

  1. concentrationThe reaction was concentrated to dryness
  2. dissolutionthe residue was dissolved in tetrahydrofuran (8 mL)
  3. temperatureThe solution was cooled to 0° C
  4. stirringThe reaction was stirred at 0° C. for 2 hours
  5. customThe reaction was quenched with saturated ammonium chloride
  6. additionThe mixture was diluted with dichloromethane and water
  7. customThe layers were separated
  8. extractionthe aqueous was extracted again with dichloromethane
  9. dry with materialThe combined organic layers were dried over sodium sulfate
  10. filtrationfiltered
  11. concentrationconcentrated
  12. customPurification by column chromatography

출처 및 근거

ORD 기록
ord-fae16057e6634b10a1c1ee887528a470
출처 데이터셋
uspto-grants-2015_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08933104B2

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