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2-Bromo-N-methyl-N-phenylacetamide → HCID 14855467、化合物

HRID 477391
ノート
印刷プレビュー

反応式

HRID 477391 の反応式
[Na].[F:2][C:3]([F:14])([C:8]1[CH:12]=[C:11]([OH:13])[O:10][N:9]=1)[C:4]([F:7])([F:6])[F:5].[CH3:15][N:16]([C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)[C:17](=[O:20])[CH2:18]Br>C(#N)C>[CH3:15][N:16]([C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)[C:17](=[O:20])[CH2:18][O:13][C:11]1[O:10][N:9]=[C:8]([C:3]([F:2])([F:14])[C:4]([F:7])([F:6])[F:5])[CH:12]=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

4

反応物 2

HCID 344952-Bromo-N-methyl-N-phenylacetamideHCID 178516125HCID 178516125、化合物

生成物 1

HCID 14855467HCID 14855467、化合物収率 67.5%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

反応条件

温度
60 °C

実験手順

To 0.50 g (2.2 mmole) of 3-pentafluoroethyl-5-hydroxyisoxazole sodium salt were added dry acetonitrile (7 ml) and N-methyl-N-phenyl-2-bromoacetamide (0.55 g) and the resulting mixture was stirred at 60° C. for 24 hours. After completion of reaction, the reaction solution was evaporated under reduced pressure and to the residue was added water (80 ml), extracted with methylene chloride, treated with anhydrous sodium sulfate and concentrated under reduced pressure. The residue was purified by chromatography on silica gel to give 0.52 g of crystals. These crystals were recrystallized from n-hexane to give 0.48 g of the titled compound as colorless plates, yield 62.3%, m.p. 88.0-89.0° C.

後処理

  1. customAfter completion of reaction
  2. customthe reaction solution was evaporated under reduced pressure and to the residue
  3. additionwas added water (80 ml)
  4. extractionextracted with methylene chloride
  5. additiontreated with anhydrous sodium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was purified by chromatography on silica gel

出典と根拠

ORDレコード
ord-ebc78d76f1ca42829655549d9ef96307
出典データセット
uspto-grants-1989_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04888044

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート