m-Chloroperbenzoic acid → HCID 86607018、化合物

HRID 1293454ノート

反応式

HRID 1293454 の反応式
[Cl:1][C:2]1[CH:3]=[N:4][CH:5]=[C:6]([Cl:26])[C:7]=1[NH:8][C:9]([C:11]1[C:19]2[C:18]3[CH:20]=[CH:21][CH:22]=[CH:23][C:17]=3[O:16][C:15]=2[C:14]([O:24][CH3:25])=[CH:13][CH:12]=1)=[O:10].ClC1C=CC=C(C(OO)=[O:35])C=1>C(Cl)(Cl)Cl>[Cl:26][C:6]1[CH:5]=[N:4][CH:3]=[C:2]([Cl:1])[C:7]=1[NH+:8]([O-:35])[C:9]([C:11]1[C:19]2[C:18]3[CH:20]=[CH:21][CH:22]=[CH:23][C:17]=3[O:16][C:15]=2[C:14]([O:24][CH3:25])=[CH:13][CH:12]=1)=[O:10]

参加物

4

反応物 2

HCID 70297m-Chloroperbenzoic acidHCID 98431931-Dibenzofurancarboxamide, N-(3,5-dichloro-4-pyridinyl)-4-methoxy-

生成物 1

HCID 86607018HCID 86607018、化合物収率 71.8%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

A suspension of N-(3,5-dichloropyrid-4-yl)-4-methoxy dibenzo[b,d]furan-1-carboxamide (200 mg, 0.518 mmol) (example 1) and m-chloroperbenzoic acid (50-55%) (880 mg, 2.5 mmol) in chloroform (10 ml) was refluxed for 2 h. The reaction was cooled and washed with saturated sodium bicarbonate and water. The organic solvent was distilled of in vacuo and the residue was purified by column chromatography using 20% acetone-chloroform as the eluent to give 150 mg of N-(3,5-dichloropyrid-4-yl)-4-methoxy dibenzo[b,d]furan-1-carboxamide-N1-oxide as white solid; mp: 265-270° C.

後処理

  1. temperaturewas refluxed for 2 h
  2. temperatureThe reaction was cooled
  3. washwashed with saturated sodium bicarbonate and water
  4. distillationThe organic solvent was distilled of in vacuo
  5. customthe residue was purified by column chromatography

出典と根拠

ORDレコード
ord-7aac8013dd5e4e94b8ae21f83c7b0156
出典データセット
uspto-grants-2007_07
特許番号
US07238725B2

反応ノート

読み込み中…