Water → Methyl 2-chloro-5-fluoro-6-methoxynicotinate

HRID 1510681ノート

反応式

HRID 1510681 の反応式
[Cl:1][C:2]1[N:11]=[C:10](Cl)[C:9]([F:13])=[CH:8][C:3]=1[C:4]([O:6][CH3:7])=[O:5].C[O-].[Na+].CO.O.[C:20](OCC)(=[O:22])C>CO>[Cl:1][C:2]1[N:11]=[C:10]([O:22][CH3:20])[C:9]([F:13])=[CH:8][C:3]=1[C:4]([O:6][CH3:7])=[O:5]

参加物

6

反応物 4

HCID 962WaterHCID 8857Ethyl AcetateHCID 2775354Methyl 2,6-dichloro-5-fluoronicotinateHCID 23694274Sodium methanolate methanol

生成物 1

HCID 40148026Methyl 2-chloro-5-fluoro-6-methoxynicotinate

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

To a solution of 1.5 g of methyl 2,6-dichloro-5-fluoronicotinate in 12 mL of methanol, a solution of 1.3 g of 28% sodium methoxide/methanol in 3 mL of methanol was dropped, and the mixture was stirred at room temperature for 40 minutes. Thereto were added water and ethyl acetate, the organic layer was separated, and the aqueous layer was extracted with ethyl acetate. The organic layer and the extract were combined, the resultant solution was washed with water and a saturated aqueous sodium chloride solution and dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure to obtain 1.2 g of methyl 2-chloro-5-fluoro-6-methoxynicotinate as a white solid.

後処理

  1. customthe organic layer was separated
  2. extractionthe aqueous layer was extracted with ethyl acetate
  3. washthe resultant solution was washed with water
  4. dry with materiala saturated aqueous sodium chloride solution and dried over anhydrous magnesium sulfate
  5. distillationthe solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-4cda4a63888c4641b2b2a84dccf1ae56
出典データセット
uspto-grants-2012_07
特許番号
US08211908B2

反応ノート

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