Ethanol → [1,1'-Biphenyl]-4-amine, 3-nitro-

HRID 480509

反応式

HRID 480509 の反応式
[OH-].[K+].[N+:3]([C:6]1[CH:7]=[C:8]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[CH:9]=[CH:10][C:11]=1[NH:12]C(=O)C)([O-:5])=[O:4].C(O)C>O>[N+:3]([C:6]1[CH:7]=[C:8]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[CH:9]=[CH:10][C:11]=1[NH2:12])([O-:5])=[O:4]

参加物

5

反応物 3

HCID 702EthanolHCID 14797Potassium HydroxideHCID 79364Acetamide, N-(3-nitro(1,1'-biphenyl)-4-yl)-2 回

生成物 1

HCID 77705[1,1'-Biphenyl]-4-amine, 3-nitro-収率 71.8%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

A mixture of potassium hydroxide (2.5 g), 3-nitro-4-acetamido-1,1′-biphenyl (23.5 g), prepared in (A) above, water (6 mL) and ethanol (12 mL) is heated at reflux for one hour. The reaction mixture is cooled to room temperature and then poured into 300 mL of a mixture of water and ice. The solid is collected by filtration and the crude product is recrystallized from methanol (800 mL) to give 14.1 g of the title compound as an orange solid melting at 170-172° C.

後処理

  1. temperatureis heated
  2. temperatureat reflux for one hour
  3. filtrationThe solid is collected by filtration
  4. customthe crude product is recrystallized from methanol (800 mL)

出典と根拠

ORDレコード
ord-1530f57a55bb4b08a15376989465a1e8
出典データセット
uspto-grants-2003_11
特許番号
US06649770B1

関連ノート

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