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Water → HCID 12084324, 화합물

HRID 1744746
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HRID 1744746 반응식
Br[CH2:2][CH2:3][CH2:4][CH3:5].[F:6][C:7]1[C:19]2[CH2:18][C:17]3[C:12](=[CH:13][CH:14]=[CH:15][C:16]=3[F:20])[C:11]=2[CH:10]=[CH:9][C:8]=1[OH:21].C(=O)([O-])[O-].[K+].[K+].O>CC(=O)CC>[CH2:2]([O:21][C:8]1[CH:9]=[CH:10][C:11]2[C:12]3[C:17](=[C:16]([F:20])[CH:15]=[CH:14][CH:13]=3)[CH2:18][C:19]=2[C:7]=1[F:6])[CH2:3][CH2:4][CH3:5]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 8002Butyl bromideHCID 11430Potassium CarbonateHCID 22223132HCID 22223132, 화합물

생성물 1

HCID 12084324HCID 12084324, 화합물

시약·촉매·용매 1

HCID 6569Methyl Ethyl Ketone용매

실험 절차

56 mmol of 1-bromobutane are added to a mixture of 36 mmol of 1,8-difluorofluoren-2-ol and 109 mmol of anhydrous potassium carbonate in 250 ml of 2-butanone (methyl ethyl ketone) and the mixture is subsequently heated to reflux for 8 h. The still hot solution is then mixed with 50 ml of water. The phases are separated, the organic phase is washed with water and saturated sodium chloride solution and dried over sodium sulfate, and the solvent is removed on a rotary evaporator. The purification is effected by filtration through aluminum oxide (neutral) using toluene as the eluent and recrystallization from heptane. 2-Butoxy-1,8-difluorofluorene is obtained.

후처리

  1. temperaturethe mixture is subsequently heated
  2. temperatureto reflux for 8 h
  3. customThe phases are separated
  4. washthe organic phase is washed with water and saturated sodium chloride solution
  5. dry with materialdried over sodium sulfate
  6. customthe solvent is removed on a rotary evaporator
  7. customThe purification
  8. filtrationis effected by filtration through aluminum oxide (neutral)
  9. customas the eluent and recrystallization from heptane

출처 및 근거

ORD 기록
ord-b2a77374c890483eb4eb9baea7bf7f33
출처 데이터셋
uspto-grants-2006_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07018685B2

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