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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Fluorene → 1-Bromo-9h-fluorene

HRID 7194
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인쇄 미리보기

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HRID 7194 반응식
[CH:1]1[C:13]2[CH2:12][C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]=2[CH:4]=[CH:3][CH:2]=1.[Br:14]N1C(=O)CCC1=O>C1(=O)OC(C)CO1>[Br:14][C:1]1[C:13]2[CH2:12][C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]=2[CH:4]=[CH:3][CH:2]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 6853FluoreneHCID 67184N-bromobutanimide

생성물 1

HCID 186948301-Bromo-9h-fluorene수율 68%

시약·촉매·용매 1

HCID 7924Propylene Carbonate용매

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온도
80 °C

실험 절차

1.2 litters of propylene carbonate and 160 g (0.96 mol) of fluorene were put into a 2 litter 3-neck round-bottom flask equipped with a stirrer, a thermometer and a reflux condenser under an argon atmosphere, and the resulting mixture was heated to 80° C. so as to make completely dissolved. 179.9 g (1.01 mol) of N-bromosuccinimide was added portionwise to the reaction mixture, and the resultant was stirred at 80° C. for 10 hours. The reaction mixture was cooled down to room temperature to precipitate white solid. The solid was filtered, thoroughly washed with methanol, dried and then recrystallized from ethanol, to obtain white crystal, which was filtered and then sufficiently dried in a vacuum oven at 40° C. to give 160 g (yield: 60%) of the desired product, and its melting point was 102° C.–103° C.

후처리

  1. customequipped with a stirrer
  2. dissolutionto make completely dissolved
  3. temperatureThe reaction mixture was cooled down to room temperature
  4. customto precipitate white solid
  5. filtrationThe solid was filtered
  6. washthoroughly washed with methanol
  7. customdried
  8. customrecrystallized from ethanol
  9. customto obtain white crystal, which
  10. filtrationwas filtered
  11. customsufficiently dried in a vacuum oven at 40° C.

출처 및 근거

ORD 기록
ord-a37453ac498b403e8ea58f83bd8e7af0
출처 데이터셋
uspto-grants-2006_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07084231B2

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