関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | 4-chloro-1-methyl-1H-imidazo(4,5-c)pyridine | HCID 948792 | — |
| 反応物 | Sodium hydrogen sulfide hydrate | HCID 53442613 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1-Methyl-1,5-dihydro-imidazo[4,5-c]pyridine-4-thione | HCID 19353598 | 95% |
反応手順
4.00 g (23.9 mmol) of 4-chloro-1-methyl-1H-imidazo[4,5-c]pyridine in 27 ml of dimethylformamide were stirred at 115° C. for 18 hours with 8.10 g (95.6 mmol) of sodium hydrogen sulphide hydrate. After cooling the mixture was treated with 110 ml of water, adjusted to pH 4 with acetic acid and stirred at 5° C. while cooling with ice for 15 min. The precipitate was filtered off and washed with water. After drying there were obtained 3.73 g (95%) of 1-methyl-1,5-dihydro-imidazo[4,5-c]pyridine-4-thione as white crystals with m.p.>300° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06030984 |
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| 出典データセット | uspto-grants-2000_02 |
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| ORD ID | ord-255934d2907e40d1a13faa0e50e75060 |
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| 出典メモ | uspto-grants-2000_02 |
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