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Toluene → HCID 22146252, 화합물

HRID 1823701
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HRID 1823701 반응식
[CH3:1][CH:2]([CH2:17][CH3:18])[CH2:3][O:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[O:11][CH2:12][CH:13]([CH3:16])[CH2:14][CH3:15].C(#N)C.[Br:22]N1C(=O)CCC1=O.C1(C)C=CC=CC=1>O>[CH3:1][CH:2]([CH2:17][CH3:18])[CH2:3][O:4][C:5]1[CH:10]=[C:9]([Br:22])[CH:8]=[CH:7][C:6]=1[O:11][CH2:12][CH:13]([CH3:16])[CH2:14][CH3:15]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 1140TolueneHCID 6342Acetonitrile2회HCID 67184N-bromobutanimideHCID 22146239HCID 22146239, 화합물

생성물 1

HCID 22146252HCID 22146252, 화합물

시약·촉매·용매 1

HCID 962Water용매

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온도
0 °C

실험 절차

1,2-Bis(2-methylbutyloxy)benzene (338 g, 1.35 mol) together with 2.5 l of acetonitrile was placed in a reaction vessel, cooled to 0° C. and admixed with 264 g (1.48 mol) of N-bromosuccinimide. The mixture was warmed to RT and stirred for another 90 minutes. After taking off the acetonitrile, the residue was admixed with toluene and water and the phases were separated. After shaking the aqueous phase with toluene and drying the organic phase over Na2SO4, the toluene was taken off. The crude product was purified by double fractional distillation under reduced pressure. This gave the product as a colorless oil (145° C., 1.3 mbar): 275 g (62%).

후처리

  1. temperatureThe mixture was warmed to RT
  2. customthe phases were separated
  3. stirringAfter shaking the aqueous phase with toluene
  4. dry with materialdrying the organic phase over Na2SO4
  5. distillationThe crude product was purified by double fractional distillation under reduced pressure

출처 및 근거

ORD 기록
ord-4e6c824e384947cba43c6849e5aab398
출처 데이터셋
uspto-grants-2006_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07041388B1

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