참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Methylamine | HCID 6329 | — |
| 반응물 | Tetrahydrofuran | HCID 8028 | — |
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | PyBOP | HCID 2724699 | — |
| 반응물 | 2-Chloropyrimidine-4-carboxylic acid | HCID 22135751 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | HCID 86669127 | HCID 86669127 | — |
반응 단계
2-Chloropyrimidine-4-carboxylic acid (Maybridge Chemicals, Maybridge, UK, 0.523 g, 3.30 mmol), DIPEA (0.48 mL, 2.75 mmol) and PyBop (1.717 g, 3.30 mmol) were weighed into a 150 mL round bottomed flask and dissolved in dioxane (15 mL). The solution was stirred at RT, then cooled to 0° C., and stirred for 5 min. Methylamine, 2.0 M in THF (2.75 mL, 5.50 mmol) was added, and the solution became a thick suspension. The suspension was stirred at 0° C. for 2.5 h. No further progression was seen, so an additional equivalent of MeNH2 was added, and the mixture was stirred for another 4 h. EtOAc was added and the mixture was washed with water (50 mL), 1 N NaOH (2×50 mL) and brine (50 mL). The material was dried over MgSO4, filtered and concentrated and used without purification. MS (ESI, pos. ion) m/z: 171.9 (M+H)+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US09321756B2 |
|---|
| 출처 데이터셋 | uspto-grants-2016_04 |
|---|
| ORD ID | ord-51a410a0c52c4181baebf9d1b7b8d4f0 |
|---|
| 출처 메모 | uspto-grants-2016_04 |
|---|