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Water → 2-Phenyl-4-(2,6-difluorophenyl)oxazole

HRID 1738380
ノート
印刷プレビュー

反応式

HRID 1738380 の反応式
[F:1][C:2]1[CH:11]=[CH:10][CH:9]=[C:8]([F:12])[C:3]=1[C:4](=O)[CH2:5]Br.[C:13]([NH2:21])(=[O:20])[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1.O>CC1C=CC=CC=1C>[C:14]1([C:13]2[O:20][CH:5]=[C:4]([C:3]3[C:2]([F:1])=[CH:11][CH:10]=[CH:9][C:8]=3[F:12])[N:21]=2)[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 962WaterHCID 2331BenzamideHCID 27782632,6-Difluorophenacyl bromide

生成物 1

HCID 217155952-Phenyl-4-(2,6-difluorophenyl)oxazole収率 121.8%

試薬・触媒・溶媒 1

HCID 7237O-Xylene溶媒

実験手順

5.7 g 2,6-difluorophenacyl bromide and 3.63 g benzamide were suspended in 20 ml o-xylene, and the suspension was subjected to reflux under heating for 1.5 hours. After completing the reaction, the suspension reacted was added with water, then extracted with ethyl acetate and further washed with saturated saline solution. The organic layer obtained was dried with anhydrous magnesium sulfate, and the solvent used was removed by distillation under reduced pressure. Out of 7.6 g residue obtained, 1.0 g thereof was purified by using silica gel column chromatography, affording the objective substance in an amount of 0.6 g.

後処理

  1. temperatureto reflux
  2. temperatureunder heating for 1.5 hours
  3. customthe reaction
  4. customthe suspension reacted
  5. extractionextracted with ethyl acetate
  6. washfurther washed with saturated saline solution
  7. customThe organic layer obtained
  8. dry with materialwas dried with anhydrous magnesium sulfate
  9. customthe solvent used was removed by distillation under reduced pressure

出典と根拠

ORDレコード
ord-0924e2a4ac5e421595e2eb83470635df
出典データセット
uspto-grants-1999_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05962685

反応ノート

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