Methyl Salicylate → HCID 9250987、化合物

HRID 2399277ノート

反応式

HRID 2399277 の反応式
[C:1]([O:10][CH3:11])(=[O:9])[C:2]1[C:3](=[CH:5][CH:6]=[CH:7][CH:8]=1)[OH:4].Cl[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=1[N+:19]([O-:21])=[O:20].C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[N+:19]([C:14]1[CH:15]=[CH:16][CH:17]=[CH:18][C:13]=1[O:4][C:3]1[CH:5]=[CH:6][CH:7]=[CH:8][C:2]=1[C:1]([O:10][CH3:11])=[O:9])([O-:21])=[O:20]

参加物

5

反応物 3

HCID 4133Methyl SalicylateHCID 69451-Chloro-2-nitrobenzeneHCID 11430Potassium Carbonate

生成物 1

HCID 9250987HCID 9250987、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

Methyl salicylate (1.7 mL, 0.0131 mol), 1-chloro-2-nitrobenzene (2.30 mL, 0.01965 mol) and potassium carbonate (3.62 g, 0.0262 mol) were mixed in dimethylformamide (35 mL), under argon, at 150° C. for 16 h. The solvent was evaporated and the crude material was flash chromatographed (silica gel, ethyl acetate/hexane). Concentration in vacuo yielded the title compound. 1H NMR (250 MHz, CDCl3) δ8.0 (m, 4H), 7.58 (m, 1H), 7.35 (m, 1H), 7.23 (m, 1H), 7.13 (dd, 1H), 6.85 (dd, 2H).

後処理

  1. customThe solvent was evaporated
  2. customchromatographed (silica gel, ethyl acetate/hexane)
  3. concentrationConcentration in vacuo

出典と根拠

ORDレコード
ord-11314236eab64891bef81af358e843c9
出典データセット
uspto-grants-1995_09
特許番号
US05447957

反応ノート

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