関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methanethiol | HCID 878 | — |
| 反応物 | 4-Methoxy-6-methylpyrimidin-2-amine | HCID 587236 | — |
| 反応物 | Methyl (2-chlorobenzene-1-sulfonyl)carbamodithioate | HCID 13364655 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 溶媒 | O-Xylene | HCID 7237 | — |
| 生成物 | N-(2-chlorophenylsulfonyl)-N'-(4-methoxy-6-methyl-2-pyrimidinyl) thiourea | HCID 14275697 | 84.7% |
反応手順
A solution of 5.0 g of methyl N-(2-chlorophenylsulfonyl)dithiocarbamate in 20 ml of xylene is stirred for 3.5 hours with heating at 145° C. During the heating, methylmercaptan gas is generated. After the reaction is completed, xylene is removed under reduced pressure to yield a pale yellow oil (IR: strong absorption band of -SO2NCS at 1900 cm-1). The oily substance is dissolved in 50 ml of acetonitrile, to which 2.8 g of 2-amino-4-methoxy-6-methylpyrimidine is added and stirred for 30 minutes at 50° C. The precipitated crystals are collected by filtration, and recrystallized from acetonitrile to give 5.6 g of the title compound as a white prism. mp 186.5°~187.5° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04897105 |
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| 出典データセット | uspto-grants-1990_01 |
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| ORD ID | ord-03289b2be8f149a7808885c2de492294 |
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| 出典メモ | uspto-grants-1990_01 |
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