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Methyl 6-formylpyridine-3-carboxylate → HCID 67980582、化合物

HRID 2406949
ノート
印刷プレビュー

反応式

HRID 2406949 の反応式
[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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

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

生成物 1

HCID 67980582HCID 67980582、化合物収率 39.2%

試薬・触媒・溶媒 2

HCID 3007855Zincchloride触媒HCID 8028
Tetrahydrofuran
溶媒

反応条件

温度
90 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-b1f06747736541a5b962b6c9e63ad8db
出典データセット
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08809342B2

反応ノート

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