참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 2,6-Diacetylpyridine | HCID 70790 | — |
| 반응물 | 2-Chloro-4,6-dimethylaniline | HCID 113033 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 2,6-Bis[1-(2-chloro-4,6-dimethylphenylimino)ethyl]pyridine | HCID 58097740 | 74.7% |
반응 단계
To a solution of 2,6-diacetylpyridine (35 g, 0.21 mol) in THF (1.21) was added 2-chloro-4,6-dimethylaniline (76.7 g, 2.3 eq) and Sicapent (45 g). The reaction mixture was refluxed overnight. Then additional 2-chloro-4,6-dimethylaniline (25 g, 0.7 eq) and Sicapent (25 g) were added and once again refluxed overnight. The suspension was cooled to 22° C., filtered and washed with two times THF (75 ml). The mother liquor was concentrated (90%) and methanol was added to precipitate the product, which was washed two times with methanol (50 ml) and dried under high vacuum. 68.8 g of a yellow powder was isolated (y=73.1%)
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08759460B2 |
|---|
| 출처 데이터셋 | uspto-grants-2014_06 |
|---|
| ORD ID | ord-afeb893ab894431d89fb4142e79dd804 |
|---|
| 출처 메모 | uspto-grants-2014_06 |
|---|