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Ammonia → Ethyl 3-amino-4-methyl-pent-2-enoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | p-Toluenesulfonic acid | HCID 6101 | — |
| 反応物 | Ethyl isobutyrylacetate | HCID 81583 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | Ethyl 3-amino-4-methyl-pent-2-enoate | HCID 59557418 | — |
反応手順
10.8 g of p-toluenesulphonic acid×4 H2O are added to 500 g (3.16 mol) of ethyl isobutyrylacetate in 1,500 ml of toluene p.a., the mixture is saturated with ammonia gas while stirring at room temperature and allowed to stand overnight. It is then heated under reflux in a water separator and ammonia gas is continuously introduced until the calculated amount of water has separated (47 ml of water after reflux for 8 hours). The mixture is allowed to cool overnight, and the precipitate which has deposited is filtered off with suction and washed with toluene. The combined toluene phases are washed several times with water, dried using sodium sulphate, concentrated in vacuo and distilled in a high vacuum.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05418243 |
| 出典データセット | uspto-grants-1995_05 |
| ORD ID | ord-df9dac4e3ee44848a058c685983c1cf1 |
| 出典メモ | uspto-grants-1995_05 |