関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | 1,2-Dichloroethylene | HCID 10900 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2-Pyrrolidinone, 1-(hydroxymethyl)- | HCID 84911 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-Chloro-3-(2-oxopyrrolidin-1-yl)propanal | HCID 53629163 | — |
反応手順
In a 250 ml, three-necked flask fitted with a magnetic stirrer, 1-(hydroxymethyl)pyrrolidin-2-one x82 (15 g, 0.13 mol) is cooled to −10° C. Cold concentrated sulfuric acid (150 ml) is added dropwise. At this temperature, 1,2-dichloroethene (46.73 g, 0.482 mol) is added while the temperature is kept below 0° C. At the end of the addition the mixture is stirred at 40° C. for 2 h. Water is added and the pH is adjusted with K2CO3. The aqueous phase is extracted with CH2Cl2, the combined organic phases are dried over MgSO4, filtered and concentrated. The crude 2-chloro-3-(2-oxopyrrolidin-1-yl)propanal x83 is used in the next step without any further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08518943B2 |
|---|
| 出典データセット | uspto-grants-2013_08 |
|---|
| ORD ID | ord-bb9515b5a4394681a0b7360f5cfcf5e3 |
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| 出典メモ | uspto-grants-2013_08 |
|---|
