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

HRID 586678
ノート
印刷プレビュー

反応式

HRID 586678 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6422Trifluoroacetic acidHCID 8053Isoamyl NitriteHCID 4124402Phosphinic AcidHCID 22335738HCID 22335738、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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:

後処理

  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

出典と根拠

ORDレコード
ord-55a2fa4ef75c41aa96be375c7753a323
出典データセット
uspto-grants-2005_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06936636B2

反応ノート

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