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Carbon tetrabromide → HCID 12606990, 화합물

HRID 341756
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HRID 341756 반응식
[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
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

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

생성물 1

HCID 12606990HCID 12606990, 화합물수율 258.8%

시약·촉매·용매 2

HCID 11776Triphenylphosphine촉매HCID 1049Pyridine
용매

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온도
0 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-c2962ddc9659493684557a5774eb4c15
출처 데이터셋
uspto-grants-1999_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05856273

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