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

HRID 2382116ノート

反応式

HRID 2382116 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-c614821056c248cf81d3702b9e6e3c91
出典データセット
uspto-grants-2012_09
特許番号
US08258130B2

反応ノート

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