반응식
[OH:1]OS([O-])=O.[K+].[CH3:7][S:8][C:9]1[CH:16]=[CH:15][C:12]([C:13]#[N:14])=[CH:11][CH:10]=1.[OH2:17]>CO>[CH3:7][S:8]([C:9]1[CH:16]=[CH:15][C:12]([C:13]#[N:14])=[CH:11][CH:10]=1)(=[O:1])=[O:17]참가 물질
5
실험 절차
A solution of oxone (18.42 g, 0.03 mol) in water (70 ml) was added dropwise to the vigorous stirred solution of 4-methylthiobenzonitrile (1.49 g, 0.01 mol) in methanol (50 ml) at 20° C. and stirring was continued for three hours. The reaction mixture was diluted with water (50 ml) and extracted with ethyl acetate. The ethyl acetate extract was washed with water, dried over anhydrous sodium sulphate and concentrated under reduced pressure to finish the title compound (1.3 g, 72.2%), mp 145-149° C. The compound was used with out any purification for the next step. 1H-NMR (CDCl3):δ 3.1 (s, 3H), 7.8-7.9 (d, 2H), 8.08-8.1 (d, 2H).
후처리
- extractionextracted with ethyl acetate
- extractionThe ethyl acetate extract
- washwas washed with water
- dry with materialdried over anhydrous sodium sulphate
- concentrationconcentrated under reduced pressure
- customThe compound was used with out any purification for the next step
출처 및 근거
- ORD 기록
- ord-e49c99a73935496d9b326a44e8837331
- 출처 데이터셋
- uspto-grants-2008_04
- 특허 번호
- US07365069B2
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