関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | HCID 66783496 | HCID 66783496 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 4-(3-Piperidin-1-yl-propyl)-[1,4]diazepan-5-one dihydrochloride | HCID 67080747 | — |
反応手順
A solution of 7.3 g (21.50 mmol) of 5-oxo-4-(3-piperidin-1-yl-propyl)-[1,4]diazepane-1-carboxylic acid tert-butyl ester was dissolved in 140 ml CH2Cl2, cooled to 0° C. and treated with 54 ml (215.03 mmol) of 4M HCl in dioxane, then warmed to RT. After 3 h, 40 ml of MeOH were added to dissolve the precipitation and stirring was continued over night. The solution was evaporated, dissolved in toluene and evaporated (2×) to yield 7.71 g (quantitative) of the title compound as a white solid. MS: 240.1 (MH+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07632829B2 |
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| 出典データセット | uspto-grants-2009_12 |
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| ORD ID | ord-6f5c80cb758041f7b03a362c62d0a878 |
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| 出典メモ | uspto-grants-2009_12 |
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