참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Diethyl Ether | HCID 3283 | — |
| 반응물 | 1-Tetralone | HCID 10724 | — |
| 반응물 | Sodium ethoxide | HCID 2723922 | — |
| 반응물 | N-(dimethylamino-3-ethoxycarbonylpropenylidene)-N-methylmethanaminium tetrafluoroborate | HCID 86743575 | — |
| 용매 | Ethanol | HCID 702 | — |
| 생성물 | Diisopropyl Ether | HCID 7914 | — |
| 생성물 | HCID 53777110 | HCID 53777110 | 33.5% |
반응 단계
α-Tetralone (51 g) is added dropwise in the course of 45 minutes, at a temperature in the region of 15° C., to a mixture of N-(3-dimethylamino-3-ethoxycarbonylpropenylidene)-N-methylmethanaminium tetrafluoroborate (100 g) in ethanol (500 cc) and a 2M ethanolic solution of sodium ethylate (210 cc). The mixture is maintained for 1 hour 45 minutes at a temperature in the region of 20° C. and is then heated for 4 hours 45 minutes to 70° C. The reaction ethanol is evaporated off to dryness and the oil obtained is pounded with ethyl ether (4×300 cc). The ethereal extracts are concentrated to dryness under reduced pressure (20 mm Hg; 2.7 kPa). After recrystallization of the solid obtained in a boiling mixture (60 cc) of isopropyl ether and ethyl acetate (90:10 by volume), ethyl 2-dimethylamino-4-(1-oxo-1,2,3,4-tetrahydro-2-naphthylidene)-2-butenoate (17.5 g), m.p. 84° C., is obtained.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US04886835 |
|---|
| 출처 데이터셋 | uspto-grants-1989_12 |
|---|
| ORD ID | ord-9c589d637e044b4ea5c51eaf5dac36c2 |
|---|
| 출처 메모 | uspto-grants-1989_12 |
|---|