2-Chlorophenol → HCID 3432930, 화합물

HRID 1464444노트

반응식

HRID 1464444 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 3432930HCID 3432930, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
65 °C

실험 절차

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.

후처리

  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.

출처 및 근거

ORD 기록
ord-c7d56218c9d04584ad870404ed4d4f20
출처 데이터셋
uspto-grants-1994_04
특허 번호
US05304644

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