Water → 4'-Amino-6-methyl-N-[3-(trifluoromethyl)phenyl]biphenyl-3-carboxamide

HRID 1894883ノート

反応式

HRID 1894883 の反応式
[CH3:1][C:2]1[C:7]([C:8]2[CH:13]=[CH:12][C:11]([N+:14]([O-])=O)=[CH:10][CH:9]=2)=[CH:6][C:5]([C:17]([NH:19][C:20]2[CH:25]=[CH:24][CH:23]=[C:22]([C:26]([F:29])([F:28])[F:27])[CH:21]=2)=[O:18])=[CH:4][CH:3]=1.O1CCOCC1.O.[OH-].[NH4+].S(S([O-])=O)([O-])=O.[Na+].[Na+].NC1C=CC=CC=1>>[NH2:14][C:11]1[CH:12]=[CH:13][C:8]([C:7]2[C:2]([CH3:1])=[CH:3][CH:4]=[C:5]([C:17]([NH:19][C:20]3[CH:25]=[CH:24][CH:23]=[C:22]([C:26]([F:27])([F:28])[F:29])[CH:21]=3)=[O:18])[CH:6]=2)=[CH:9][CH:10]=1

参加物

7

反応物 6

HCID 962WaterHCID 6115AnilineHCID 14923Ammonium HydroxideHCID 24489Sodium DithioniteHCID 312751,4-DioxaneHCID 690428606-Methyl-4'-nitro-N-[3-(trifluoromethyl)phenyl]biphenyl-3-carboxamide

生成物 1

HCID 690431094'-Amino-6-methyl-N-[3-(trifluoromethyl)phenyl]biphenyl-3-carboxamide

反応条件

温度
25 °C

実験手順

6-Methyl-4′-nitro-N-[3-(trifluoromethyl)phenyl]biphenyl-3-carboxamide was dissolved in 1,4-dioxane (10.00 mL, 0.1281 mol) and water (5.00 mL, 0.278 mol), and ammonium hydroxide (0.18 mL, 0.0045 mol) was added. To the reaction was added sodium dithionite (1.10 g, 0.00632 mol) and this mixture was stirred at 25° C. for 2 hours at which time HPLC analysis showed aniline formation. The reaction was extracted with ethyl acetate and the organic extracts were washed with water, saturated NaCl, dried (MgSO4) and concentrated in vacuo. MS (EI) m/z=371 (M+H).

後処理

  1. extractionThe reaction was extracted with ethyl acetate
  2. washthe organic extracts were washed with water, saturated NaCl
  3. dry with materialdried (MgSO4)
  4. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-1fcedce4e3c04c45a9efd8a4a77f8d19
出典データセット
uspto-grants-2013_08
特許番号
US08513270B2

反応ノート

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