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Carbon tetrabromide → HCID 12606990、化合物

HRID 341756
ノート
印刷プレビュー

反応式

HRID 341756 の反応式
[F:1][C:2]([F:14])([F:13])[C:3]1[CH:4]=[C:5]([NH:9][CH2:10][CH2:11]O)[CH:6]=[CH:7][CH:8]=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(Br)(Br)(Br)[Br:35]>N1C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>[Br:35][CH2:11][CH2:10][NH:9][C:5]1[CH:6]=[CH:7][CH:8]=[C:3]([C:2]([F:14])([F:13])[F:1])[CH:4]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 11205Carbon tetrabromideHCID 11776TriphenylphosphineHCID 156361032-((3-(Trifluoromethyl)phenyl)amino)ethanol

生成物 1

HCID 12606990HCID 12606990、化合物収率 258.8%

試薬・触媒・溶媒 2

HCID 11776Triphenylphosphine触媒HCID 1049Pyridine
溶媒

反応条件

温度
0 °C

実験手順

N-(3-trifluoromethylphenyl)ethanolamine (4.17 g) and triphenyl phosphine (5.50 g) were dissolved in dry pyridine (35 ml) and stirred at 0° C. To this solution was added, portionwise, carbon tetrabromide (7.08 g). Stirring was continued for 1 hour and the reaction mixture was left to stand at room temperature overnight. A little more triphenyl phosphine (0.20 g) was added, and when virtually all starting alcohol had been consumed the pyridine was removed under reduced pressure to leave a brown residue (14.10 g). This was chromatographed on silica gel, eluting with ethyl acetate/hexane (1:9) as eluant to give the title compound as a light brown oil, yield 3.35 g.

後処理

  1. additionTo this solution was added
  2. stirringStirring
  3. waitthe reaction mixture was left
  4. waitto stand at room temperature overnight
  5. customwhen virtually all starting alcohol had been consumed the pyridine
  6. customwas removed under reduced pressure

出典と根拠

ORDレコード
ord-c2962ddc9659493684557a5774eb4c15
出典データセット
uspto-grants-1999_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05856273

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート