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3-Nitroaniline → 4'-Trifluoromethyl-biphenyl-2-carboxylic acid (3-nitro-phenyl)-amide

HRID 51974
ノート
印刷プレビュー

反応式

HRID 51974 の反応式
[N+:1]([C:4]1[CH:5]=[C:6]([CH:8]=[CH:9][CH:10]=1)[NH2:7])([O-:3])=[O:2].C(N(CC)CC)C.[F:18][C:19]([F:36])([F:35])[C:20]1[CH:25]=[CH:24][C:23]([C:26]2[C:27]([C:32](Cl)=[O:33])=[CH:28][CH:29]=[CH:30][CH:31]=2)=[CH:22][CH:21]=1>C1COCC1>[N+:1]([C:4]1[CH:5]=[C:6]([NH:7][C:32]([C:27]2[C:26]([C:23]3[CH:24]=[CH:25][C:20]([C:19]([F:18])([F:35])[F:36])=[CH:21][CH:22]=3)=[CH:31][CH:30]=[CH:29][CH:28]=2)=[O:33])[CH:8]=[CH:9][CH:10]=1)([O-:3])=[O:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 74233-Nitroaniline2 回HCID 8471TriethylamineHCID 110660004'-(Trifluoromethyl)-[1,1'-biphenyl]-2-carbonyl chloride

生成物 1

HCID 101569574'-Trifluoromethyl-biphenyl-2-carboxylic acid (3-nitro-phenyl)-amide収率 100%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a solution of 3-nitroaniline (28.8 g, 209 mmol, 1 equiv) in THF (1000 mL, 35 volumes), was added triethylamine (70 mL, 500 mmol, 2.4 equiv). 3-Nitroaniline can be obtained from Aldrich, Milwaukee, Wis. A solution of 4′-trifluoromethyl-biphenyl-2-carbonyl chloride (71.3 g, 250 mmol, 1.2 equiv) in THF (250 mL, 3.5 volumes) was added dropwise over 30 minutes. The reaction was stirred at room temperature for 48 hours. The slurry was then filtered through diatomaceous earth and the filtrate was concentrated. Water (700 mL, 24 volumes) was added and the slurry was stirred at room temperature for 12 hours. The solids were collected by filtration and dried under vacuum at 40° C. to provide 4′-trifluoromethyl-biphenyl-2-carboxylic acid (3-nitro-phenyl)-amide (80.7 g, 100%) as a pale yellow powder.

後処理

  1. filtrationThe slurry was then filtered through diatomaceous earth
  2. concentrationthe filtrate was concentrated
  3. additionWater (700 mL, 24 volumes) was added
  4. stirringthe slurry was stirred at room temperature for 12 hours
  5. filtrationThe solids were collected by filtration
  6. customdried under vacuum at 40° C.

出典と根拠

ORDレコード
ord-2927607f630a4bbc812d4fbdab602dd2
出典データセット
uspto-grants-2004_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06713489B2

反応ノート

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