関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Formaldehyde | HCID 712 | — |
| 反応物 | Spermidine | HCID 1102 | — |
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | Ammonium Hydroxide | HCID 14923 | — |
| 反応物 | Silica | HCID 24261 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 1-(4-Aminobutyryl)hexahydropyrmidine | HCID 22438004 | — |
反応手順
To a solution of 7.5 g of spermidine in water (150 mL) in a 250 mL round bottom flask was added paraformaldehyde (1.6 g). The resulting solution was stirred at room temperature for three hours. TLC (silicon dioxide, ethyl acetate:methanol:ammonium hydroxide=3:6:1) indicated there was no S.M. (Rf-0.01). To the reaction mixture was added toluene (100 mL). The resulting heterogeneous solution was concentrated on a rotovap at 45° C. for 30 minutes. The addition of toluene (100 mL) and concentration at 45° C. was repeated for two more times. The resulting thick oil was washed with tetrahydrofuran:ethanol (10:1)(×3) (220 mL). The combined organic layers were dried with sodium sulfate, filtered and concentrated to give 8.64 g of the title compound as a crude thick oil (yield 103%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05869734 |
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| 出典データセット | uspto-grants-1999_02 |
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| ORD ID | ord-425aecf5935a48a1a72dd8291d9952a4 |
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| 出典メモ | uspto-grants-1999_02 |
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