Methyl 4-amino-3-iodo-5-nitrobenzoate → Methyl 3,4-diamino-5-iodobenzoate

HRID 59805

反応式

HRID 59805 の反応式
[CH3:1][O:2][C:3](=[O:15])[C:4]1[CH:9]=[C:8]([N+:10]([O-])=O)[C:7]([NH2:13])=[C:6]([I:14])[CH:5]=1>C(OCC)(=O)C>[CH3:1][O:2][C:3](=[O:15])[C:4]1[CH:5]=[C:6]([I:14])[C:7]([NH2:13])=[C:8]([NH2:10])[CH:9]=1

参加物

3

反応物 1

HCID 67512142Methyl 4-amino-3-iodo-5-nitrobenzoate

生成物 1

HCID 67512100Methyl 3,4-diamino-5-iodobenzoate

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

反応条件

温度
70 °C

実験手順

To a solution of 4-amino-3-iodo-5-nitro-benzoic acid methyl ester in ethyl acetate (50 mL) was added SnCl2 dihydrate. The mixture was heated to 70° C. for two hours, then cooled to room temperature and partitioned between ethyl acetate and satruated aqueous sodium bicarbonate. The organic layer was separated, dried over MgSO4, filtered and concentrated under reduced pressure to provide 1.68 g (quantitative) of 3,4-diamino-5-iodo-benzoic acid methyl ester.

後処理

  1. temperaturecooled to room temperature
  2. custompartitioned between ethyl acetate
  3. customThe organic layer was separated
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-9459193e86ed4825aac16c791697ebcc
出典データセット
uspto-grants-2016_09
特許番号
US09440956B2

関連ノート

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