Water → 2-((2-Chloro-4-nitrophenoxy)methyl)pyridine

HRID 403655

反応式

HRID 403655 の反応式
[OH-].[K+].[N:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[CH2:9][OH:10].[Cl:11][C:12]1[CH:13]=[C:14]([N+:19]([O-:21])=[O:20])[CH:15]=[CH:16][C:17]=1F.O>C(#N)C>[Cl:11][C:12]1[CH:13]=[C:14]([N+:19]([O-:21])=[O:20])[CH:15]=[CH:16][C:17]=1[O:10][CH2:9][C:4]1[CH:5]=[CH:6][CH:7]=[CH:8][N:3]=1

参加物

6

反応物 4

HCID 962WaterHCID 11474PiconolHCID 14797Potassium HydroxideHCID 676882-Chloro-1-fluoro-4-nitrobenzene

生成物 1

HCID 174694332-((2-Chloro-4-nitrophenoxy)methyl)pyridine収率 69.6%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒2 回

反応条件

温度
35 °C

実験手順

A mixture of potassium hydroxide (20.6 g, 0.15 mol, 0.52 equiv) and 2-pyridylcarbinol (31.08 g, 0.285 mol, 1.00 equiv) in acetonitrile (750 ml) was stirred at 35° C. for 30 minutes. A solution of the 3-chloro-4-fluoronitrobenzene (50 g, 0.29 mol, 1.00 equiv) in acetonitrile (250 ml) was added and the mixture was stirred at 40° C. for 14 hours and then cooled to room temperature. Water (1000 ml) was added and the precipitated solids were filtered and washed with water and dried to give product 52.5 g. MS (ESI) m/z: 265 (M+1).

後処理

  1. stirringthe mixture was stirred at 40° C. for 14 hours
  2. temperaturecooled to room temperature
  3. filtrationthe precipitated solids were filtered
  4. washwashed with water
  5. customdried

出典と根拠

ORDレコード
ord-d3f649813b384047864f8537d31e75db
出典データセット
uspto-grants-2014_06
特許番号
US08748453B2

関連ノート

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