Ethyl orthoformate → HCID 66847930、化合物

HRID 475428ノート

反応式

HRID 475428 の反応式
[Br:1][C:2]1[CH:18]=[CH:17][C:5]2[C:6]([C:9]3[CH:16]=[CH:15][CH:14]=[CH:13][C:10]=3C=O)=[N:7][O:8][C:4]=2[CH:3]=1.[CH:19]([O:26][CH2:27][CH3:28])([O:23][CH2:24][CH3:25])OCC>C(O)C.C1(C)C=CC(S(O)(=O)=O)=CC=1>[Br:1][C:2]1[CH:18]=[CH:17][C:5]2[C:6]([C:9]3[CH:16]=[CH:15][CH:14]=[CH:13][C:10]=3[CH:19]([O:23][CH2:24][CH3:25])[O:26][CH2:27][CH3:28])=[N:7][O:8][C:4]=2[CH:3]=1

参加物

5

反応物 2

HCID 31214Ethyl orthoformateHCID 866759952-(6-Bromobenzo[d]isoxazol-3-yl)benzaldehyde2 回

生成物 1

HCID 66847930HCID 66847930、化合物収率 101.2%

試薬・触媒・溶媒 2

HCID 6101p-Toluenesulfonic acid触媒HCID 702Ethanol溶媒

反応条件

温度
45 °C

実験手順

To a stirred suspension of 2-(6-bromobenzo[d]isoxazol-3-yl)benzaldehyde (Compound 4a) (10 g) in dry ethanol (100 mL) was added p-toluenesulfonic acid (0.315 g) followed by triethyl orthoformate (11.01 mL, 9.81 g). The suspension was stirred at 45° C. until a clear solution resulted and then maintained at 45° C. for 45 min. The solvent was removed under vacuum and then the mixture was diluted with ethyl acetate and then washed with saturated sodium carbonate solution, brine and then dried over anhydrous sodium sulfate, filtered and evaporated to give the title product (12.6 g).

後処理

  1. customresulted
  2. temperaturemaintained at 45° C. for 45 min
  3. customThe solvent was removed under vacuum
  4. additionthe mixture was diluted with ethyl acetate
  5. washwashed with saturated sodium carbonate solution, brine
  6. dry with materialdried over anhydrous sodium sulfate
  7. filtrationfiltered
  8. customevaporated

出典と根拠

ORDレコード
ord-75172dc3bc1f4a749e9bfecad9efacab
出典データセット
uspto-grants-2014_01
特許番号
US08637551B2

反応ノート

読み込み中…