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Formaldehyde → 1-Hydroxymethyl-3-(1-methyl-4-piperidinyl)-1H-indazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Formaldehyde | HCID 712 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | HCID 178480237 | HCID 178480237 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 1-Hydroxymethyl-3-(1-methyl-4-piperidinyl)-1H-indazole | HCID 14032504 | 57.8% |
反応手順
A solution of 0.52 g of paraformaldehyde, 3.0 g of 3-(1-methyl-4-piperidinyl)-1H-indazole, 15 ml of ethanol and 0.34 ml of 5% aqueous sodium hydroxide was refluxed for 3 hrs. The ethanol was removed in vacuo and the residue diluted with water. The aqueous suspension was extracted with dichloromethane (2x, 50 ml) and the combined extracts were washed with water and dried over anhydrous magnesium sulfate. The dichloromethane was evaporated in vacuo to yield an oil, which crystallized upon standing. The solid was recrystallized twice from ethyl acetate to yield 1.3 g (57.8%) of product, mp 128°-130° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04710573 |
| 出典データセット | uspto-grants-1987_12 |
| ORD ID | ord-2cbc01f5374b4d74bd0aee0b14a5c6c3 |
| 出典メモ | uspto-grants-1987_12 |