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Propargylamine → HCID 178457562、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Propargylamine | HCID 239041 | — |
| 反応物 | HCID 178503877 | HCID 178503877 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | HCID 178457562 | HCID 178457562 | 116.4% |
反応手順
A mixture of N-cyano-N'-{2-[(4-methyl-5-imidazolyl)methylthio]ethyl}-S-methyl isothiourea (3.00 g, 0.0111 mole) and propargyl amine (2.50 g, 0.045 mole) in acetonitrile (60 ml) as stirred at reflux for 65 hours, and then was heated in a stainless steel pressure vessel at 120°-130° for 38 hours. The reaction mixture was cooled, decanted from a tar, and then evaporated to leave a gum (3.57 g). This material was placed on silica gel (100-200 mesh) and eluted with a mixture of methylene chloride (97 parts) and methanol (3 parts). The product obtained from a middle fraction was crystallized by trituration under acetonitrile, and then was recrystallized from acetonitrile to yield the title compound (0.236 g; 7.7%); m.p. 146°-149.5°.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | USRE031588 |
| 出典データセット | uspto-grants-1984_05 |
| ORD ID | ord-c416bf9d832f40ec990391cabaeb4b17 |
| 出典メモ | uspto-grants-1984_05 |