참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Acetonitrile | HCID 6342 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | Ethyl cyclopentanecarboxylate | HCID 79550 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | 3-Cyclopentyl-3-oxopropanenitrile | HCID 13592118 | — |
반응 단계
To a suspension of sodium hydride (350 mg, 8.8 mmol, 1.2 eq) in 1,4-dioxane (10 mL) was added acetonitrile (450 μL, 8.8 mmol, 1.2 eq). The mixture was stirred at room temperature for 30 min. Then cyclopentanecarboxylic acid ethyl ester (660 μL, 7.3 mmol, 1 eq) was added. After stirring for 30 min at room temperature, the mixture was heated at 105° C. during 16 h. After cooling, the solvent was evaporated to dryness and water was added (30 mL). The mixture was extracted with dichloromethane (3×30 mL) to get rid of the starting material and the aqueous phase was acidified with a 1N solution of hydrochloric acid and extracted with dichloromethane (3×30 mL). The combined organic phases were dried over magnesium sulfate, filtered and dried in vacuo to afford 3-cyclopentyl-3-oxo-propionitrile as very volatile yellow oil (1.0 g, quant. yield)
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US09434745B2 |
|---|
| 출처 데이터셋 | uspto-grants-2016_09 |
|---|
| ORD ID | ord-50d04bc57d8d493bbf86638150ebe891 |
|---|
| 출처 메모 | uspto-grants-2016_09 |
|---|