참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Diethylamine | HCID 8021 | — |
| 반응물 | Cyanocyclohexane | HCID 69834 | — |
| 반응물 | Ethane, 2-bromo-1,1-diethoxy- | HCID 74852 | — |
| 반응물 | Butyllithium | HCID 178418339 | — |
| 용매 | Hexane | HCID 8058 | — |
| 생성물 | 1-(2,2-Diethoxyethyl)cyclohexane-1-carbonitrile | HCID 13217350 | — |
반응 단계
51.7 ml (0.5 mol) of anhydrous diethylamine are added dropwise to 312.5 ml (0.5 mol) of a 15% solution of n-butyl-lithium in hexane at -10° C. under an inert gas blanket. The batch is stirred for 10 minutes and then cooled to -70° C. Within 30 minutes, 54.6 g of cyclohexane-carbonitrile are added dropwise, after a further 30 minutes 98.5 g of bromoacetaldehyde-diethylacetal are added within 1 hour, and the batch is maintained for 24 hours at low temperature. Subsequently, it is warmed to room temperature, given onto 100 g of ice, extracted twice with 500 ml of ethyl acetate, the organic phase is dried over sodium sulfate, concentrated in vacuo, and the residue is subjected to vacuum distillation.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US04515960 |
|---|
| 출처 데이터셋 | uspto-grants-1985_05 |
|---|
| ORD ID | ord-26fc452980d64f33bffc69f7d14a2f3a |
|---|
| 출처 메모 | uspto-grants-1985_05 |
|---|