5-(2-Chloro-5-(trifluoromethyl)phenoxy)-2-nitropyridine → 5-(2-Chloro-5-(trifluoromethyl)phenoxy)pyridin-2-amine

HRID 2272171ノート

反応式

HRID 2272171 の反応式
[Cl:1][C:2]1[CH:17]=[CH:16][C:15]([C:18]([F:21])([F:20])[F:19])=[CH:14][C:3]=1[O:4][C:5]1[CH:6]=[CH:7][C:8]([N+:11]([O-])=O)=[N:9][CH:10]=1>C(O)C.ClCCl.[Pd]>[Cl:1][C:2]1[CH:17]=[CH:16][C:15]([C:18]([F:19])([F:21])[F:20])=[CH:14][C:3]=1[O:4][C:5]1[CH:6]=[CH:7][C:8]([NH2:11])=[N:9][CH:10]=1

参加物

4

反応物 1

HCID 671268785-(2-Chloro-5-(trifluoromethyl)phenoxy)-2-nitropyridine

生成物 1

HCID 671269145-(2-Chloro-5-(trifluoromethyl)phenoxy)pyridin-2-amine収率 96.3%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 21584144Dichloromethane ethanol溶媒

実験手順

10% Pd/C (38 mg, 35 μmol, 10 mol % Pd) was added to chloride 3 (113 mg, 353 μmol) in ethanol:dichloromethane (3:1, 4.0 mL). The mixture was degassed and placed under H2 (1 atm) and stirred for 1 h. The mixture, filtered through a 0.45 μm syringe filter and concentrated under reduced pressure provided 4 (98.1 mg, 96%) as a solid: LRESIMS m/z 289.4 [M+H]+, calcd. for C12H9Cl1F3N2O1 289.0.

後処理

  1. customThe mixture was degassed
  2. filtrationThe mixture, filtered through a 0.45 μm syringe
  3. filtrationfilter
  4. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-37cfb3c261fc48b599fc738aefe90059
出典データセット
uspto-grants-2015_09
特許番号
US09120751B2

反応ノート

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