Diiodomethane → 26516-42-7

HRID 333476

반응식

HRID 333476 반응식
[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]

참가 물질

3

반응물 2

HCID 6346DiiodomethaneHCID 690702,6-Dinitroaniline

생성물 1

HCID 1457118426516-42-7수율 52%

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-e76a131dc89948efa60069429aeef6a7
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08877905B2

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