Potassium Carbonate → 2-(2,4-Difluorophenyl)oxirane

HRID 880617

反応式

HRID 880617 の反応式
[BH4-].[Na+].Br[CH2:4][C:5]([C:7]1[CH:12]=[CH:11][C:10]([F:13])=[CH:9][C:8]=1[F:14])=[O:6].C([O-])([O-])=O.[K+].[K+]>CO>[F:14][C:8]1[CH:9]=[C:10]([F:13])[CH:11]=[CH:12][C:7]=1[CH:5]1[CH2:4][O:6]1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 27741852-Bromo-2',4'-difluoroacetophenoneHCID 4311764Sodium borohydride

生成物 1

HCID 143729242-(2,4-Difluorophenyl)oxirane

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Sodium borohydride (0.367 g, 10.85 mmol) was added to a stirred solution of 2-bromo-2′,4′-difluoroacetophenone ([CAS 102429-07-2], 5.1 g, 21.7 mmol) in MeOH (152 mL) at 10° C. The mixture was stirred at RT for 1 h. Then, K2CO3 (4.499 g, 32.55 mmol) was added and the mixture was stirred at RT for 1 h. The mixture was filtered through diatomaceous earth and the filtrate was concentrated in vacuo. The residue was treated with water and extracted with CH2Cl2/THF. The organic layer was separated, dried (Na2SO4), filtered and the solvents evaporated in vacuo to yield I-19 (2.24 g, 66%) as a yellow oil.

後処理

  1. stirringthe mixture was stirred at RT for 1 h
  2. filtrationThe mixture was filtered through diatomaceous earth
  3. concentrationthe filtrate was concentrated in vacuo
  4. additionThe residue was treated with water
  5. extractionextracted with CH2Cl2/THF
  6. customThe organic layer was separated
  7. dry with materialdried (Na2SO4)
  8. filtrationfiltered
  9. customthe solvents evaporated in vacuo
  10. customto yield I-19 (2.24 g, 66%) as a yellow oil

出典と根拠

ORDレコード
ord-cda5a70adcba496dbcc8fc946b69d1c3
出典データセット
uspto-grants-2015_03
特許番号
US08993591B2

関連ノート

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