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Phosphorus oxide (P4O10) → 2-(4-Bromophenyl)oxazole

HRID 396781
ノート
印刷プレビュー

反応式

HRID 396781 の反応式
[Br:1][C:2]1[CH:18]=[CH:17][C:5]([C:6]([NH:8][CH2:9][CH:10]([O:14]CC)OCC)=O)=[CH:4][CH:3]=1.O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O.C([O-])(O)=O.[Na+].[NH4+].[OH-]>S(=O)(=O)(O)O>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([C:6]2[O:14][CH:10]=[CH:9][N:8]=2)=[CH:17][CH:18]=1
参加物反応条件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 14812Phosphorus oxide (P4O10)HCID 14923Ammonium HydroxideHCID 516892Sodium BicarbonateHCID 223168934-bromo-N-(2,2-diethoxyethyl)benzamide

生成物 1

HCID 110750322-(4-Bromophenyl)oxazole収率 70%

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid
溶媒
2 回

反応条件

温度
180 °C

実験手順

4-Bromo-N-(2,2-diethoxyethyl)benzamide was dissolved in concentrated sulfuric acid at 0° C. To phosphorus pentoxide (5.2 g, 18.3 mmol) was added the sulfuric acid solution, and the mixture was heated at 180° C. for 30 minutes. The reaction mixture was cooled down to room temperature, and poured into ice. The whole was made basic by addition of NaHCO3 and ammonia aqueous solution. The whole was extracted with ethyl acetate. The organic layer was washed with brine, dried over MgSO4, and concentrated in vacuo to give title compound (1.23 g, 70% yield).

後処理

  1. temperatureThe reaction mixture was cooled down to room temperature
  2. additionpoured into ice
  3. extractionThe whole was extracted with ethyl acetate
  4. washThe organic layer was washed with brine
  5. dry with materialdried over MgSO4
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-78e73b92e1f140aca7ee94768131eb3c
出典データセット
uspto-grants-2003_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06608095B2

反応ノート

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