1,2-Dichlorobenzene → 1-Fluoro-2-nitronaphthalene

HRID 2379460

반응식

HRID 2379460 반응식
[F:1][B-](F)(F)F.N#[O+].N[C:9]1[C:18]2[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=2)[CH:12]=[CH:11][C:10]=1[N+:19]([O-:21])=[O:20].ClC1C=CC=CC=1Cl>ClCCl>[F:1][C:9]1[C:18]2[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=2)[CH:12]=[CH:11][C:10]=1[N+:19]([O-:21])=[O:20]

참가 물질

5

반응물 3

HCID 72391,2-DichlorobenzeneHCID 1364032-Nitronaphthalen-1-amineHCID 11137142Nitrilooxonium tetrafluoroborate

생성물 1

HCID 220084711-Fluoro-2-nitronaphthalene

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a well stirred slurry of nitrosonium tetrafluoroborate (Aldrich) (10 % molar excess, (cf. David J. Milner, Synthetic Communications (1992) 22 (1), 73-82.)) in dichloromethane at 0° C. is added 1-amino-2-nitronaphthalene. After 30 minutes, ortho-dichlorobenzene is added and the dichloromethane is distilled off, and the dichlorobenzene is heated at 50°-200 ° C. to decompose the diazonium tetrafluoroborate. Removal of solvent and purification of the product by chromatography or crystallization yields 1-fluoro-2-nitronaphthalene.

후처리

  1. distillationthe dichloromethane is distilled off
  2. temperaturethe dichlorobenzene is heated at 50°-200 ° C.
  3. customRemoval of solvent and purification of the product
  4. customby chromatography or crystallization

출처 및 근거

ORD 기록
ord-d9497c760e6047559109574ac42038e4
출처 데이터셋
uspto-grants-1994_11
특허 번호
US05362747

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