참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 3,4,5-Trimethoxybenzonitrile | HCID 15892 | — |
| 반응물 | 2-Methylnicotinic acid | HCID 643373 | — |
| 반응물 | Lithium diisopropylamide | HCID 2724682 | — |
| 반응물 | Methanedione--ethanol (1/1) | HCID 19604758 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | HCID 178487380 | HCID 178487380 | — |
반응 단계
7 g 2-Methyl-nicotinic acid was suspended in 150 mL of tetrahydrofuran, and cooled to −70° C. with a bath of ethanol/dry ice. 80 mL lithium diisopropylamide (2.0 M in tetrahydrofuran/n-heptane/ethylbenzene) was added dropwise over 10 min and the mixture was stirred for 2 h at 0° C. Then it was cooled to −73° C. and a solution of 10 g 3,4,5-trimethoxy-benzonitrile (4.24) in 50 mL tetrahydrofuran was added. Then the reaction mixture was warmed overnight to ambient temperature. 30 mL Water was added and the solvent was distilled off before 200 mL ethyl acetate was added and the precipitate that formed was collected.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US09187478B2 |
|---|
| 출처 데이터셋 | uspto-grants-2015_11 |
|---|
| ORD ID | ord-6323fba206c947c0ab6d6554ac4e6c86 |
|---|
| 출처 메모 | uspto-grants-2015_11 |
|---|
