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Trifluoroacetic acid → 2-Bromo-1,4-bis(propan-2-yl)benzene

HRID 586678
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반응식

HRID 586678 반응식
FC(F)(F)C(O)=O.C([C:11]1([Br:21])[CH:16]=[CH:15][CH:14]=[C:13]([CH:17]([CH3:19])[CH3:18])[CH:12]1N)(C)C.[CH2:22](ON=O)[CH2:23][CH:24](C)C.O[PH2]=O>CCO>[CH:23]([C:16]1[CH:15]=[CH:14][C:13]([CH:17]([CH3:18])[CH3:19])=[CH:12][C:11]=1[Br:21])([CH3:24])[CH3:22]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 6422Trifluoroacetic acidHCID 8053Isoamyl NitriteHCID 4124402Phosphinic AcidHCID 22335738HCID 22335738, 화합물

생성물 1

HCID 119589802-Bromo-1,4-bis(propan-2-yl)benzene

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Trifluoroacetic acid (75 mL was added to a solution of Intermediate 34 in EtOH (100 mL) at 0° C. After stirring for 10 min, iso-amylnitrite (100 mL) was then added and the mixture was stirred for another 70 min. H3PO2 (70 mL) was added slowly and the mixture was warmed to ambient temperature over 5 hours. After dilution with ethyl acetate and sodium bicarbonate solution, the organic layer was separated, dried and concentrated to give the title compound in a crude form (17 g). Purification of the crude product by Kugelrohr distillation gave the title compound in pure form (13 g, 44% yield over 4 steps from 1,3-di-iso-propyl-benzene) as a colorless oil:

후처리

  1. stirringthe mixture was stirred for another 70 min
  2. customAfter dilution with ethyl acetate and sodium bicarbonate solution, the organic layer was separated
  3. customdried
  4. concentrationconcentrated

출처 및 근거

ORD 기록
ord-55a2fa4ef75c41aa96be375c7753a323
출처 데이터셋
uspto-grants-2005_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06936636B2

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