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HRID 257856作成日:2026年10月25日

Amidosulfenyl chloride, N,N-dibutyl- → N-(N,N-di-n-butylaminosulfenyl)-N-[4-(4-methylthiophenoxy)benzyl]4-chloro-1,3-dimethylpyrazole-5-carboxamide

https://huagongshe.com/reaction/257856

反応式

関与物質

役割名称HCID仕込み量
反応物Amidosulfenyl chloride, N,N-dibutyl-HCID 81031—
反応物N-[4-(4-methylthiophenoxy)benzyl]-4-chloro-1,3-dimethylpyrazole-5-carboxamideHCID 131717883—
触媒4-(Dimethylamino)pyridineHCID 14284—
溶媒PyridineHCID 1049—
生成物N-(N,N-di-n-butylaminosulfenyl)-N-[4-(4-methylthiophenoxy)benzyl]4-chloro-1,3-dimethylpyrazole-5-carboxamideHCID 13171788252%

反応手順

To a stirred mixture of N-[4-(4-methylthiophenoxy)benzyl]-4-chloro-1,3-dimethylpyrazole-5-carboxamide (300 mg, 0.746 mM), 4-(N,N-dimethylamino)pyridine (119 mg, 0.970 mM) and dry pyridine (5 ml) was added dropwise N,N-di-n-butylaminosulfenyl chloride (190 mg, 0.970 mM) at 0°-10° C., and the mixture was stirred for 4 h at the room temperature. The mixture was poured into ice water, and the mixture was extracted with dichloromethane. The extract was washed with saturated ammonium chloride solution(x2) and brine, dried with sodium sulfate, and concentrated in vacuo. The residue was chromatographed over silica gel to give N-(N,N-di-n-butylaminosulfenyl)-N-[4-(4-methylthiophenoxy)benzyl]4-chloro-1,3-dimethylpyrazole-5-carboxamide (217 mg, 52%) as a colorless oil, nD23.3 1.5748.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US05264448
出典データセットuspto-grants-1993_11
ORD IDord-70575816ce5b448e86c03a55f380eb2e
出典メモuspto-grants-1993_11