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

HRID 38506

반응식

HRID 38506 반응식
[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

참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 1140Toluene용매HCID 8857Ethyl Acetate용매

반응 조건

온도
60 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-69410e23ead34d7c983e71982da85b2a
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08524722B2

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