Methyl 2-iodo-3-nitrobenzoate → Methyl 3-amino-2-iodobenzoate

HRID 1639833

反応式

HRID 1639833 の反応式
[I:1][C:2]1[C:11]([N+:12]([O-])=O)=[CH:10][CH:9]=[CH:8][C:3]=1[C:4]([O:6][CH3:7])=[O:5]>[Ni].C(OCC)(=O)C>[NH2:12][C:11]1[C:2]([I:1])=[C:3]([CH:8]=[CH:9][CH:10]=1)[C:4]([O:6][CH3:7])=[O:5]

参加物

4

反応物 1

HCID 264093Methyl 2-iodo-3-nitrobenzoate

生成物 1

HCID 18340005Methyl 3-amino-2-iodobenzoate収率 86.3%

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 8857Ethyl Acetate溶媒

実験手順

A mixture of methyl 2-iodo-3-nitrobenzoate (77.0 g, 251 mmol) and a catalytic amount of Raney nickel in ethyl acetate (100 mL) was stirred under hydrogen atmosphere at room temperature for 2 days, and filtered through celite. The solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane=1/10) to give the title compound (60.0 g, yield 86%).

後処理

  1. filtrationfiltered through celite
  2. customThe solvent was evaporated under reduced pressure
  3. customThe residue was purified by silica gel column chromatography (ethyl acetate/hexane=1/10)

出典と根拠

ORDレコード
ord-ce1864c71942400885a878c44086a9e2
出典データセット
uspto-grants-2012_02
特許番号
US08110585B2

関連ノート

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