HCID 23031086、化合物 → HCID 23031257、化合物

HRID 1766676ノート

反応式

HRID 1766676 の反応式
FC(F)(F)S(O[C:7]1[C:15]([CH3:16])=[CH:14][C:13]([N+:17]([O-:19])=[O:18])=[C:12]2[C:8]=1[CH2:9][CH2:10][CH2:11]2)(=O)=O.O.[I-:23].[Li+]>CN(C)C=O>[I:23][C:7]1[C:15]([CH3:16])=[CH:14][C:13]([N+:17]([O-:19])=[O:18])=[C:12]2[C:8]=1[CH2:9][CH2:10][CH2:11]2

参加物

4

反応物 2

HCID 23031086HCID 23031086、化合物HCID 23688290LITHIUM IODIDE

生成物 1

HCID 23031257HCID 23031257、化合物収率 77.8%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
150 °C

実験手順

To a solution of 5-methyl-7-nitroindan-4-yl trifluoromethanesulfonate (3.02 g) in N,N-dimethylformamide (10 mL) was added lithium iodide mono hydrate (6.10 g). The mixture was stirred under an argon atmosphere at 150° C. for 7 hours. Adding water, the reaction mixture was extracted with ethyl acetate. The organic layer was washed with a 1 mol/L aqueous solution of sodium hydroxide, water and brine successively, and dried over anhydrous magnesium sulfate. The solvent was removed under reduced pressure to give the title compound (2.19 g).

後処理

  1. extractionAdding water, the reaction mixture was extracted with ethyl acetate
  2. washThe organic layer was washed with a 1 mol/L aqueous solution of sodium hydroxide, water and brine successively
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customThe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-d7861d79d19e4ebb8d3744b70f930fe5
出典データセット
uspto-grants-2007_06
特許番号
US07230031B2

反応ノート

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