関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Cyclohexane, (bromomethyl)- | HCID 137636 | — |
| 反応物 | 2-(2-Methyl-4-nitrophenylimino)-3-thia-1-azaspiro[4.4]nonane | HCID 178428736 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1-(Cyclohexylmethyl)-2-(2-methyl-4-nitrophenylimino)-3-thia-1-azaspiro[4.4]nonane | HCID 18316077 | 32% |
反応手順
To a solution of 2-(2-methyl-4-nitrophenylimino)-3-thia-1-azaspiro[4.4]nonane (Method C2a; 0.10g, 0.3432 mmol) and bromomethylcyclohexane (1.00 mL) in DMF (1.00 mL) was added NaOH (approx. 0.13 g). The resulting mixture was stirred at 45° C. for 2 d during which it turned from deep red to bright orange. The reaction mixture was then cooled to room temp., filtered and concentrated under reduced pressure. The residual oil was purified by chromatography (SiO2; 5% EtOAc/hex) to afford 1-(cyclohexylmethyl)-2-(2-methyl-4-nitrophenylimino)-3-thia-1-azaspiro[4.4]nonane (0.042 g, 32%) mp 85-7° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06353006B1 |
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| 出典データセット | uspto-grants-2002_03 |
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| ORD ID | ord-9be90650ac23408a99f66696544e0098 |
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| 出典メモ | uspto-grants-2002_03 |
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