Ethyl orthoformate → HCID 66847930, 화합물

HRID 475428노트

반응식

HRID 475428 반응식
[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

참가 물질

5

반응물 2

HCID 31214Ethyl orthoformateHCID 866759952-(6-Bromobenzo[d]isoxazol-3-yl)benzaldehyde2회

생성물 1

HCID 66847930HCID 66847930, 화합물수율 101.2%

시약·촉매·용매 2

HCID 6101p-Toluenesulfonic acid촉매HCID 702Ethanol용매

반응 조건

온도
45 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-75172dc3bc1f4a749e9bfecad9efacab
출처 데이터셋
uspto-grants-2014_01
특허 번호
US08637551B2

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