반응식
[Cl:1][C:2]1[CH:3]=[C:4]([CH:7]=[C:8]([Cl:10])[N:9]=1)[CH:5]=[O:6].C1(C)C=CC(S([CH2:20][N+:21]#[C-:22])(=O)=O)=CC=1.C(=O)([O-])[O-].[K+].[K+]>CO>[Cl:1][C:2]1[CH:3]=[C:4]([C:5]2[O:6][CH:22]=[N:21][CH:20]=2)[CH:7]=[C:8]([Cl:10])[N:9]=1참가 물질
5
반응 조건
- 온도
- 50 °C
실험 절차
528 mg of 2,6-dichloroisonicotinaldehyde (this compound was prepared by the method described in J. Chem. Soc., Chem. Commun., 1998, 1567-1568) was dissolved in 10 ml of methanol, and 586 mg of p-toluenesulfonyl methyl isocyanide and 415 mg of potassium carbonate ware added, and the mixture was stirred at 50° C. for 30 minutes. The reaction solution was concentrated, and then diluted with ethyl acetate, and the organic layer was washed with a saturated aqueous solution of sodium bicarbonate and brine, and then dried over magnesium sulfate. The solvent was distilled off under reduced pressure to obtain 630 mg of the objective compound as white powder.
후처리
- concentrationThe reaction solution was concentrated
- additiondiluted with ethyl acetate
- washthe organic layer was washed with a saturated aqueous solution of sodium bicarbonate and brine
- dry with materialdried over magnesium sulfate
- distillationThe solvent was distilled off under reduced pressure
출처 및 근거
- ORD 기록
- ord-544006946f2649d186b590ddf0aa1e14
- 출처 데이터셋
- uspto-grants-2013_11
- 특허 번호
- US08586591B2
연결된 노트
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