Pyridine → Methanesulfonamide, N-phenyl-
반응식
[NH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.N1C=CC=CC=1.[CH3:14][S:15](Cl)(=[O:17])=[O:16]>C(Cl)Cl>[C:2]1([NH:1][S:15]([CH3:14])(=[O:17])=[O:16])[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1참가 물질
5
반응 조건
- 온도
- 0 °C
실험 절차
To a 0° C. solution of 250 g (2.68 mole) of aniline and 233.2 g (2.95 mole) of pyridine in 1.25 L of methylene chloride and 319.6 g (2.79 mole) of methanesulfonyl chloride dropwise. Stir the resulting solution at 0° C. for about 30 minutes then warm to ambient temperature for about 16 hours. Extract the mixture with 2N aqueous sodium hydroxide (4×1 L). Combine the aqueous extracts and wash with 1 L of methylene chloride. Cool the aqueous layer to about 0° C. and acidify with concentrated hydrochloric acid until about pH 1. Collect the precipitate and dry to give the title compound.
후처리
- customTo a 0° C.
- temperaturethen warm to ambient temperature for about 16 hours
- extractionExtract the mixture with 2N aqueous sodium hydroxide (4×1 L)
- washCombine the aqueous extracts and wash with 1 L of methylene chloride
- temperatureCool the aqueous layer to about 0° C.
- customCollect the precipitate
- customdry
출처 및 근거
- ORD 기록
- ord-fb68f984a46c4939bbfa1222749812bc
- 출처 데이터셋
- uspto-grants-1986_09
- 특허 번호
- US04613609
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