참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Methanethiol | HCID 878 | — |
| 반응물 | 4-Methoxy-6-methylpyrimidin-2-amine | HCID 587236 | — |
| 반응물 | Methyl (2-chlorobenzene-1-sulfonyl)carbamodithioate | HCID 13364655 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 용매 | O-Xylene | HCID 7237 | — |
| 생성물 | N-(2-chlorophenylsulfonyl)-N'-(4-methoxy-6-methyl-2-pyrimidinyl) thiourea | HCID 14275697 | 84.7% |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US04897105 |
|---|
| 출처 데이터셋 | uspto-grants-1990_01 |
|---|
| ORD ID | ord-03289b2be8f149a7808885c2de492294 |
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| 출처 메모 | uspto-grants-1990_01 |
|---|
