Hydrogen Peroxide → HCID 22223132、化合物

HRID 1744745ノート

反応式

HRID 1744745 の反応式
[OH:1]O.[F:3][C:4]1[C:16]2[CH2:15][C:14]3[C:9](=[CH:10][CH:11]=[CH:12][C:13]=3[F:17])[C:8]=2[CH:7]=[CH:6][C:5]=1B(O)O.O>COC(C)(C)C>[F:3][C:4]1[C:16]2[CH2:15][C:14]3[C:9](=[CH:10][CH:11]=[CH:12][C:13]=3[F:17])[C:8]=2[CH:7]=[CH:6][C:5]=1[OH:1]

参加物

5

反応物 3

HCID 784Hydrogen PeroxideHCID 962WaterHCID 22223114HCID 22223114、化合物

生成物 1

HCID 22223132HCID 22223132、化合物

試薬・触媒・溶媒 1

HCID 15413tert-Butyl methyl ether溶媒

実験手順

40 ml of hydrogen peroxide (35 percent) is added dropwise at room temperature to a suspension of 54 mmol of 1,8-difluorofluorene-2-boronic acid in 120 ml of tert-butyl methyl ether and the mixture is subsequently heated to boiling for 4 h. After cooling, the mixture is admixed with 150 ml of water, the phases are separated and the organic phase is washed twice each with water and saturated sodium sulfite solution and also with saturated sodium chloride solution, so that no more peroxide can be detected. The organic phase is dried over sodium sulfate and the solvent is removed on a rotary evaporator. Recrystallization from heptane provides 1,8-difluorofluoren-2-ol.

後処理

  1. temperaturethe mixture is subsequently heated
  2. temperatureAfter cooling
  3. customthe phases are separated
  4. washthe organic phase is washed twice each with water and saturated sodium sulfite solution
  5. dry with materialThe organic phase is dried over sodium sulfate
  6. customthe solvent is removed on a rotary evaporator
  7. customRecrystallization from heptane

出典と根拠

ORDレコード
ord-36a3a0ea83bd4aa2b38f4ae047aefa5c
出典データセット
uspto-grants-2006_03
特許番号
US07018685B2

反応ノート

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