関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Benzylamine | HCID 7504 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 5,5-Bis(bromomethyl)-2,2-dimethyl-1,3-dioxane | HCID 14537228 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | [1-Benzyl-3-(hydroxymethyl)azetidin-3-YL]methanol | HCID 20164320 | — |
反応手順
A mixture of 30.2 g of 5,5-bis(bromomethyl)-2,2-dimethyl-1,3-dioxane (0.1 mol), 24.0 g of sodium bicarbonate and 50 ml of dimethyl sulfoxide was heated to 135° C. A solution of 10.7 g of benzylamine in 50 ml of DMSO was then added dropwise with stirring over 1.5 hours. After addition was complete, the mixture was stirred for 2.5 hours at 135° C. After cooling, 100 ml of DMSO and 20 ml of water were added and the solution was extracted with pentane. The extract was washed with water and then shaken with 5% (w/w) sulfuric acid in order to extract the basic 3,3-bis(hydroxymethyl)-1-benzylazetidine acetone acetal.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04665197 |
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| 出典データセット | uspto-grants-1987_05 |
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| ORD ID | ord-42a29bca230b451e8b083a3c67f98fe8 |
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| 出典メモ | uspto-grants-1987_05 |
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