Nitric Acid → HCID 66859069、化合物

HRID 1803150ノート

反応式

HRID 1803150 の反応式
[N+:1]([O-:4])(O)=[O:2].[C:5](=[O:18])([O:15][CH2:16][CH3:17])[O:6][C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([F:13])[C:8]=1[F:14]>S(=O)(=O)(O)O>[C:5](=[O:18])([O:15][CH2:16][CH3:17])[O:6][C:7]1[CH:12]=[C:11]([N+:1]([O-:4])=[O:2])[CH:10]=[C:9]([F:13])[C:8]=1[F:14]

参加物

4

反応物 2

HCID 944Nitric AcidHCID 66858654HCID 66858654、化合物

生成物 1

HCID 66859069HCID 66859069、化合物収率 6%

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒2 回

実験手順

Step M (2): A mixture of concentrated sulfuric acid and nitric acid (1:1 ratio, 60 mL total volume) was slowly and carefully added to a solution of 2,3-difluorophenyl ethyl carbonate (20 g, 98.9 mmol) in concentrated sulfuric acid (15 mL). The internal temperature was maintained at rt throughout the addition. After complete addition, the resulting mixture was stirred for 2 h. The mixture was poured onto ice and extracted with chloroform. The organic layer was washed with brine, dried over sodium sulfate, filtered, and concentrated in vacuo. The residue was purified using silica gel column chromatography (hexane) to afford 2,3-difluoro-5-nitrophenyl ethyl carbonate (1.5 g, 6% yield).

後処理

  1. additionAfter complete addition
  2. additionThe mixture was poured onto ice
  3. extractionextracted with chloroform
  4. washThe organic layer was washed with brine
  5. dry with materialdried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo
  8. customThe residue was purified

出典と根拠

ORDレコード
ord-fcede2f1928047a58226bc08fade358b
出典データセット
uspto-grants-2013_01
特許番号
US08349880B2

反応ノート

読み込み中…