関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 3-(Trifluoromethyl)benzyl mercaptan | HCID 141236 | — |
| 反応物 | 1-Chloro-2,5-dimethyl-4-nitrobenzene | HCID 252793 | — |
| 溶媒 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 生成物 | 2-Nitro-5-(3-trifluoromethylbenzylthio)-p-xylene | HCID 22481239 | — |
反応手順
A mixture of 3-trifluoromethylbenzyl mercaptan (3.42 g), diisopropylethylamine (2.3 g) and 3-chloro-6-nitro-p-xylene (3.0 g) in dry N-methylpyrrolidinone (20 ml) was heated at 130° C. for 6 hours. On cooling, the mixture was poured into ice-water and the resulting mixture was filtered to give a solid which was washed with ice-water and then air dried. The solid was purified by silica gel chromatography eluting with light petroleum (60-80° C.)/ethyl acetate (9:1) to give the title product as a solid, m.p. 85-7° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06893650B1 |
|---|
| 出典データセット | uspto-grants-2005_05 |
|---|
| ORD ID | ord-3c5c4555a8be471c84011d0e7e10a7b2 |
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| 出典メモ | uspto-grants-2005_05 |
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