Diiodomethane → 26516-42-7

HRID 333476

反応式

HRID 333476 の反応式
[N+:1]([C:4]1[CH:10]=[CH:9][CH:8]=[C:7]([N+:11]([O-:13])=[O:12])[C:5]=1N)([O-:3])=[O:2].[I:14]CI>>[I:14][C:5]1[C:4]([N+:1]([O-:3])=[O:2])=[CH:10][CH:9]=[CH:8][C:7]=1[N+:11]([O-:13])=[O:12]

参加物

3

反応物 2

HCID 6346DiiodomethaneHCID 690702,6-Dinitroaniline

生成物 1

HCID 1457118426516-42-7収率 52%

実験手順

To a dispersion of 2,6-dinitroaniline (4.00 g, 0.021 mol) in diiodomethane (24 mL, 0.297 mol) isoamylnitrite (15 mL, 0.112 mol) was added (Smith et al., 1990, which is incorporated herein by reference). The mixture was stirred at room temperature for one hour, and then heated at 105° C. for eight hours. The excess of diiodomethane was removed in high vacuo. The residue was diluted with acetyl acetate (10 mL). Silica (ca 30 mL, mesh 230-400 Å) was added; the mixture was concentrated in vacuo and purified by column chromatography to yield 1-iodo-2,6-dinitrobenzene (3.21 g, 52%). 1H NMR (400 MHz, CDCl3): δ 7.84 (d, 2H, J=8.0 Hz), 7.67 (t, 1H, J=8.0 Hz).

後処理

  1. temperatureheated at 105° C. for eight hours
  2. customThe excess of diiodomethane was removed in high vacuo
  3. additionThe residue was diluted with acetyl acetate (10 mL)
  4. additionSilica (ca 30 mL, mesh 230-400 Å) was added
  5. concentrationthe mixture was concentrated in vacuo
  6. custompurified by column chromatography

出典と根拠

ORDレコード
ord-e76a131dc89948efa60069429aeef6a7
出典データセット
uspto-grants-2014_11
特許番号
US08877905B2

関連ノート

読み込み中…