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Methyl Ethyl Ketone → HCID 178492798、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl Ethyl Ketone | HCID 6569 | — |
| 反応物 | 3-Chloro-6-methoxypyridazine | HCID 74403 | — |
| 反応物 | Thiourea | HCID 2723790 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | HCID 178492798 | HCID 178492798 | 24% |
反応手順
A mixture of 3-chloro-6-methoxy pyridazine (0.69 mol, 100 g), thiourea (1.38 mol, 105 g) and ethyl methyl ketone (1.8 L) was refluxed for 3 hours. The reaction was cooled and the supernatant was poured into water and extracted with 1M sodium hydroxide (4×100 mL). The sodium hydroxide solution was washed with EtOAc (2×50 mL), the aqueous extract was acidified with sufficient conc. HCl to lower the pH to 5 and the resulting yellow solid was collected and air-dried to obtain 3-mercapto-6-methoxy pyridazine (24%, 23 g); mp 198° C.-200° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06849629B2 |
| 出典データセット | uspto-grants-2005_02 |
| ORD ID | ord-76473388b085410688169bdc886dcb6f |
| 出典メモ | uspto-grants-2005_02 |