Isoamyl Nitrite → 6-Fluoro-4-nitroso-3,4-dihydro-2H-benzo[1,4]oxazine

HRID 2382116노트

반응식

HRID 2382116 반응식
[N:1](OCCC(C)C)=[O:2].[F:9][C:10]1[CH:11]=[CH:12][C:13]2[O:18][CH2:17][CH2:16][NH:15][C:14]=2[CH:19]=1>C(Cl)Cl>[F:9][C:10]1[CH:11]=[CH:12][C:13]2[O:18][CH2:17][CH2:16][N:15]([N:1]=[O:2])[C:14]=2[CH:19]=1

참가 물질

4

반응물 2

HCID 8053Isoamyl NitriteHCID 162444596-Fluoro-3,4-dihydro-2H-1,4-benzoxazine

생성물 1

HCID 866393826-Fluoro-4-nitroso-3,4-dihydro-2H-benzo[1,4]oxazine

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Isoamyl nitrite is added to a solution of 6-fluoro-3,4-dihydro-2H-benzo[1,4]oxazine (1 g) in DCM (15 mL) and heated to reflux overnight. The reaction mixture is concentrated in vacuo and the residue is purified by silica gel chromatography eluting with 10% EtOAc in heptane to give 6-Fluoro-4-nitroso-3,4-dihydro-2H-benzo[1,4]oxazine (0.83 g).

후처리

  1. temperatureheated
  2. temperatureto reflux overnight
  3. concentrationThe reaction mixture is concentrated in vacuo
  4. customthe residue is purified by silica gel chromatography
  5. washeluting with 10% EtOAc in heptane

출처 및 근거

ORD 기록
ord-c614821056c248cf81d3702b9e6e3c91
출처 데이터셋
uspto-grants-2012_09
특허 번호
US08258130B2

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