Ethyl 2-fluoro-4-nitrobenzoate → Ethyl 4-Amino-2-fluorobenzoate

HRID 369774ノート

反応式

HRID 369774 の反応式
[F:1][C:2]1[CH:12]=[C:11]([N+:13]([O-])=O)[CH:10]=[CH:9][C:3]=1[C:4]([O:6][CH2:7][CH3:8])=[O:5]>CO>[CH2:7]([O:6][C:4](=[O:5])[C:3]1[CH:9]=[CH:10][C:11]([NH2:13])=[CH:12][C:2]=1[F:1])[CH3:8]

参加物

3

反応物 1

HCID 10727300Ethyl 2-fluoro-4-nitrobenzoate

生成物 1

HCID 10797532Ethyl 4-Amino-2-fluorobenzoate収率 93.1%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a 250 mL round bottomed flask equipped with a magnetic stirrer were added 3.00 g of ethyl 2-fluoro-4-nitro-benzoate and 100 mL of MeOH. The solution was deoxygenated by bubbling nitrogen through for 10 min and then treated with 2.00 g of Raney nickel (Raney 3200, Davison Chemical, Chattanooga, Tenn. 37406) which had been washed with water and EtOH. The solution was subjected to hydrogenation at 1 atm with stirring for 40 min. The flask was purged with nitrogen and the catalyst was removed by filtration. The filtrate was concentrated in vacuo to afford 2.40 g (93%) of ethyl-4-amino-2-fluorobenzoate as a tan crystalline solid, m.p. 110-112° C.

後処理

  1. customTo a 250 mL round bottomed flask equipped with a magnetic stirrer
  2. customThe solution was deoxygenated
  3. customby bubbling nitrogen through for 10 min
  4. additiontreated with 2.00 g of Raney nickel (Raney 3200, Davison Chemical, Chattanooga, Tenn. 37406) which
  5. washhad been washed with water and EtOH
  6. customThe flask was purged with nitrogen
  7. customthe catalyst was removed by filtration
  8. concentrationThe filtrate was concentrated in vacuo

出典と根拠

ORDレコード
ord-ae628b44c7e148cab5da7c8a5739309c
出典データセット
uspto-grants-2000_10
特許番号
US06140100

反応ノート

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