Ammonium formate → Ethyl 6-(3,4-difluoro phenoxy)-5-fluoronicotinate

HRID 920355ノート

反応式

HRID 920355 の反応式
C([O-])=O.[NH4+].Cl[C:6]1[N:16]=[C:15]([O:17][C:18]2[CH:23]=[CH:22][C:21]([F:24])=[C:20]([F:25])[CH:19]=2)[C:14]([F:26])=[CH:13][C:7]=1[C:8]([O:10][CH2:11][CH3:12])=[O:9]>CO.[Pd]>[F:25][C:20]1[CH:19]=[C:18]([CH:23]=[CH:22][C:21]=1[F:24])[O:17][C:15]1[C:14]([F:26])=[CH:13][C:7]([C:8]([O:10][CH2:11][CH3:12])=[O:9])=[CH:6][N:16]=1

参加物

5

反応物 2

HCID 2723923Ammonium formateHCID 86676389Ethyl 2-chloro-6-(3,4-difluorophenoxy)-5-fluoronicotinate

生成物 1

HCID 71236611Ethyl 6-(3,4-difluoro phenoxy)-5-fluoronicotinate収率 74.8%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

反応条件

温度
65 °C

実験手順

To a solution of ammonium formate (28.5 g, 452 mmol) and ethyl 2-chloro-6-(3,4-difluorophenoxy)-5-fluoronicotinate (30 g, 90 mmol) in methanol (300 mL) was added Pd/C (3 g, 2.82 mmol). The reaction mixture was stirred at 65° C. for 10 hr. and then filtered. The filtrate was concentrated under reduced pressure to get ethyl 6-(3,4-difluoro phenoxy)-5-fluoronicotinate (20 g, 48.4%).

後処理

  1. filtrationand then filtered
  2. concentrationThe filtrate was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-3feea6b5f36e407f8c5146b2e1f0957c
出典データセット
uspto-grants-2016_03
特許番号
US09273054B2

反応ノート

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