Sulfuric Acid → 1035263-42-3

HRID 2078353ノート

反応式

HRID 2078353 の反応式
[Cl:1][C:2]1[C:3]([I:11])=[C:4](CC#N)[CH:5]=[CH:6][CH:7]=1.[OH:12]S(O)(=O)=O.[O:17]1[CH2:22][CH2:21]OCC1>O>[Cl:1][C:2]1[C:3]([I:11])=[C:4]([CH2:21][C:22]([OH:17])=[O:12])[CH:5]=[CH:6][CH:7]=1

参加物

5

反応物 3

HCID 1118Sulfuric AcidHCID 312751,4-DioxaneHCID 670996963-Chloro-2-iodobenzeneacetonitrile

生成物 1

HCID 670999481035263-42-3

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
115 °C

実験手順

A mixture of 2-(3-chloro-2-iodophenyl)acetonitrile (3.2 g, 12 mmol) in 20 mL dioxane was treated with 25 mL 9M H2SO4. The mixture was stirred at 115° C. for 2 hours, cooled to room temperature, and diluted with 100 mL water. The mixture was extracted with EtOAc (3×50 mL). The combined organic layers were washed with saturated NaCl (20 mL), dried over anhydrous sodium sulfate, and concentrated to give crude product in 4 g as pale yellow solid. MS m/e: (M+H)+ 297.

後処理

  1. temperaturecooled to room temperature
  2. extractionThe mixture was extracted with EtOAc (3×50 mL)
  3. washThe combined organic layers were washed with saturated NaCl (20 mL)
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated
  6. customto give crude product in 4 g as pale yellow solid

出典と根拠

ORDレコード
ord-263baf22e1234f909d0d28d70b4a7ada
出典データセット
uspto-grants-2011_04
特許番号
US07928139B2

反応ノート

読み込み中…