Sodium Iodide → 1-Iodo-2-(3-methyl-butyl)-benzene

HRID 1436516노트

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HRID 1436516 반응식
[I-:1].[Na+].CN[C@@H]1CCCC[C@H]1NC.Br[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=1[CH2:20][CH2:21][CH:22]([CH3:24])[CH3:23]>C(O)CCCC.[Cu](I)I>[I:1][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=1[CH2:20][CH2:21][CH:22]([CH3:24])[CH3:23]

참가 물질

6

반응물 3

HCID 5238Sodium IodideHCID 2733821trans-N,N'-dimethyl-1,2-cyclohexanediamineHCID 210637691-Bromo-2-(3-methyl-butyl)-benzene

생성물 1

HCID 541304451-Iodo-2-(3-methyl-butyl)-benzene수율 84%

시약·촉매·용매 2

HCID 83717Copper iodide촉매HCID 62761-Pentanol용매2회

반응 조건

온도
130 °C

실험 절차

Charge a pressure tube with sodium iodide (734 mg, 4.9 mmol), copper iodide (23 mg, 0.12 mmol), trans-N,N′-dimethyl-cyclohexane-1,2-diamine (34 mg, 0.24 mmol) dissolved in 0.5 ml of pentanol, and 1-bromo-2-(3-methyl-butyl)-benzene dissolved in 0.5 ml of pentanol. Purge with nitrogen, cap the tube, and heat at 130° C. for 3 days. Subject to silica gel chromatography, eluting with hexane to obtain the desired compound as a colorless liquid (587 mg, 84%).

후처리

  1. customPurge with nitrogen
  2. customcap the tube
  3. washeluting with hexane

출처 및 근거

ORD 기록
ord-b98691b47b314fccb669e9c3cb4fe89c
출처 데이터셋
uspto-grants-2009_11
특허 번호
US07618978B2

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