Iodine → 4-Bromo-2-iodo-6-nitroaniline

HRID 1941917

反応式

HRID 1941917 の反応式
[Br:1][C:2]1[CH:8]=[CH:7][C:5]([NH2:6])=[C:4]([N+:9]([O-:11])=[O:10])[CH:3]=1.[I:12]I>C(O)C.S([O-])([O-])(=O)=O.[Ag+].[Ag+]>[Br:1][C:2]1[CH:3]=[C:4]([N+:9]([O-:11])=[O:10])[C:5]([NH2:6])=[C:7]([I:12])[CH:8]=1

参加物

5

反応物 2

HCID 807IodineHCID 701324-Bromo-2-nitroaniline

生成物 1

HCID 106887094-Bromo-2-iodo-6-nitroaniline収率 88%

試薬・触媒・溶媒 2

HCID 159865Silver sulfate触媒HCID 702Ethanol溶媒

実験手順

4-Bromo-2-nitroaniline (14.3 g, 0.0659 mol) was added in one portion to iodine (17.6 g, 0.0692 mol) dissolved in ethanol (300 ml), followed by silver (I) sulphate (20.4 g 0.0659 mol). After stirring at ambient temperature for 18 hours the reaction was filtered and the solid obtained was washed with dichloromethane until all the orange product had dissolved. The combined filtrates were evaporated in vacuo and the resulting solid was washed with diethyl ether/40-60 Petroleum ether (1:1) and filtered to give 4-bromo-2-iodo-6-nitroaniline as an orange solid (19.8 g, 88%), which was used without further purification.

後処理

  1. filtrationwas filtered
  2. customthe solid obtained
  3. washwas washed with dichloromethane until all the orange product
  4. dissolutionhad dissolved
  5. customThe combined filtrates were evaporated in vacuo
  6. washthe resulting solid was washed with diethyl ether/40-60 Petroleum ether (1:1)
  7. filtrationfiltered

出典と根拠

ORDレコード
ord-54557a36fd9448bfb384bda60fb8b6b2
出典データセット
uspto-grants-2013_03
特許番号
US08389516B2

関連ノート

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