3-Fluorophenol → HCID 67958741、化合物

HRID 72438

反応式

HRID 72438 の反応式
[F:1][C:2]1[CH:3]=[C:4]([OH:8])[CH:5]=[CH:6][CH:7]=1.C(=O)([O-])[O-].[K+].[K+].[Cl:15][C:16]1[CH:17]=[N:18][C:19]([N:26]2[CH2:29][CH:28](OS(C)(=O)=O)[CH2:27]2)=[C:20]([CH:25]=1)[C:21]([O:23][CH3:24])=[O:22]>C(#N)C>[Cl:15][C:16]1[CH:17]=[N:18][C:19]([N:26]2[CH2:29][CH:28]([O:8][C:4]3[CH:5]=[CH:6][CH:7]=[C:2]([F:1])[CH:3]=3)[CH2:27]2)=[C:20]([CH:25]=1)[C:21]([O:23][CH3:24])=[O:22]

参加物

5

反応物 3

HCID 97433-FluorophenolHCID 11430Potassium CarbonateHCID 86697874Methyl 5-chloro-2-(3-((methylsulfonyl)oxy)azetidin-1-yl)nicotinate

生成物 1

HCID 67958741HCID 67958741、化合物

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

反応条件

温度
180 °C

実験手順

To a solution of 3-Fluorophenol (0.005 ml, 0.056 mmole) in acetonitrile (1 ml), potassium carbonate (10 mg, 0.0728 mmol) were added followed by the addition of methyl 5-chloro-2-(3-((methylsulfonyl)oxy)azetidin-1-yl)nicotinate (D63) (20 mg, 0.062 mmol). The reaction mixture was heated at 150° C. under microwave irradiation for 10 min (2 cycle of 5 min each) then at 180° C. for 5 min. After solvent evaporation the obtained residue was purified by SPE-Si (10 g) eluting with mixture cyclohexane/ethyl acetate from 95/5 to 90/10. Collected fractions, after solvent evaporation, afforded the title compound D77 (10 mg)

後処理

  1. customAfter solvent evaporation the obtained residue
  2. customwas purified by SPE-Si (10 g)
  3. washeluting with mixture cyclohexane/ethyl acetate from 95/5 to 90/10
  4. customCollected fractions, after solvent evaporation

出典と根拠

ORDレコード
ord-87ce8322c9764f05854d307a112e4a3b
出典データセット
uspto-grants-2014_09
特許番号
US08828987B2

関連ノート

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