Water → 2-Chloro-1-(3-fluoro-benzyloxy)-4-nitro-benzene

HRID 38506

反応式

HRID 38506 の反応式
[F:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][CH:9]=1)[CH2:5][OH:6].[OH-].[K+].O.Cl[C:14]1[CH:19]=[CH:18][C:17]([N+:20]([O-:22])=[O:21])=[CH:16][C:15]=1[Cl:23]>C(OCC)(=O)C.C1(C)C=CC=CC=1>[Cl:23][C:15]1[CH:16]=[C:17]([N+:20]([O-:22])=[O:21])[CH:18]=[CH:19][C:14]=1[O:6][CH2:5][C:4]1[CH:7]=[CH:8][CH:9]=[C:2]([F:1])[CH:3]=1

参加物

7

反応物 4

HCID 962WaterHCID 74431,2-Dichloro-4-nitrobenzeneHCID 14797Potassium HydroxideHCID 680083-Fluorobenzylic alcohol

生成物 1

HCID 70592692-Chloro-1-(3-fluoro-benzyloxy)-4-nitro-benzene収率 63%

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
60 °C

実験手順

To a mixture of 3-fluorobenzyl alcohol (7.88 g, 62.5 mmol), Aliquot 336 (8.08 g, 20.0 mmol), potassium hydroxide (3.51 g, 62.5 mmol) and water (40 mL) were added toluene (80 mL) and 1,2-dichloro-4-nitrobenzene (10.0 g, 52.1 mmol). The mixture was heated to 60° C. overnight with vigorous stirring. The mixture was diluted with ethyl acetate and washed with water. The organic layer was dried over sodium sulfate, and the solvent was removed in vacuo. The residue was triturated with hot petroleum ether and tert-butyl methyl ether to yield 9.20 g (63%) of the title compound.

後処理

  1. washwashed with water
  2. dry with materialThe organic layer was dried over sodium sulfate
  3. customthe solvent was removed in vacuo
  4. customThe residue was triturated with hot petroleum ether and tert-butyl methyl ether

出典と根拠

ORDレコード
ord-69410e23ead34d7c983e71982da85b2a
出典データセット
uspto-grants-2013_09
特許番号
US08524722B2

関連ノート

読み込み中…