2-Chlorophenol → HCID 3432930、化合物

HRID 1464444ノート

反応式

HRID 1464444 の反応式
[H-].[Na+].[Cl:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[OH:10].F[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=1[N+:18]([O-:20])=[O:19]>CN(C)C=O>[Cl:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[O:10][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=1[N+:18]([O-:20])=[O:19]

参加物

5

反応物 3

HCID 72452-ChlorophenolHCID 24758Sodium hydrideHCID 738951-Fluoro-2-nitrobenzene

生成物 1

HCID 3432930HCID 3432930、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
65 °C

実験手順

Sodium hydride (1.00 g) was added in portions to a solution of 2-chlorophenol (5.00 g) in N,N-dimethylformamide (100 mL) under nitrogen. To the resulting solution was added 2-fluoro-1-nitrobenzene (5.00 g). The mixture was heated at 65° C. overnight, and then was evaporated under vacuum. The residue was partitioned between chloroform and 1 N NaOH, and the layers were separated. The aqueous layer was extracted once more with chloroform, and the combined chloroform layers were washed with water and brine, dried over magnesium sulfate, and evaporated under vacuum to a yellow oil. The oil was crystallized from ethyl ether/hexane at -78° C. to yield the title compound as a light yellow solid. Mp: 48°-49° C.

後処理

  1. customwas evaporated under vacuum
  2. customThe residue was partitioned between chloroform and 1 N NaOH
  3. customthe layers were separated
  4. extractionThe aqueous layer was extracted once more with chloroform
  5. washthe combined chloroform layers were washed with water and brine
  6. dry with materialdried over magnesium sulfate
  7. customevaporated under vacuum to a yellow oil
  8. customThe oil was crystallized from ethyl ether/hexane at -78° C.

出典と根拠

ORDレコード
ord-c7d56218c9d04584ad870404ed4d4f20
出典データセット
uspto-grants-1994_04
特許番号
US05304644

反応ノート

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