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Water → HCID 12084324、化合物

HRID 1744746
ノート
印刷プレビュー

反応式

HRID 1744746 の反応式
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]
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 962WaterHCID 8002Butyl bromideHCID 11430Potassium CarbonateHCID 22223132HCID 22223132、化合物

生成物 1

HCID 12084324HCID 12084324、化合物

試薬・触媒・溶媒 1

HCID 6569Methyl Ethyl Ketone溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b2a77374c890483eb4eb9baea7bf7f33
出典データセット
uspto-grants-2006_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07018685B2

反応ノート

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