참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Trifluoroacetic acid | HCID 6422 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | 3-amino-N-(2-(trifluoromethyl)benzyl)cyclohexanecarboxamide | HCID 59448247 | — |
| 반응물 | 4-Chloro-N-methyl-6-(4-methylpiperazin-1-yl)-1,3,5-triazin-2-amine | HCID 80767500 | — |
| 용매 | Acetonitrile--water (1/1) | HCID 18373917 | — |
| 생성물 | HCID 25118226 | HCID 25118226 | 1.8% |
반응 단계
The solution of 4-chloro-N-methyl-6-(4-methylpiperazin-1-yl)-1,3,5-triazin-2-amine (30.0 mg, 0.084 mmol, 1 equivalent) and 3-amino-N-(2-(trifluoromethyl)benzyl) cyclohexanecarboxamide as TFA salt (103 mg, 0.248 mmol, 2.95 equivalents) in CH3CN/H2O (1/1, 2 ml) was adjusted to pH 9-10 with 1N NaOH. The resulting solution was heated at 80° C. for 16 hours. The solvent was removed under vacuo to give the crude product, which was purified with RP-HPLC (Luna 5μ, C8(2), 100×21 mm, 10-50% CH3CN/H2O, 0.1% TFA, 25 min) to give the final compound (0.94 mg, 1.8%). MS (ES+): m/e 507.17 [M+H]+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US07994317B2 |
|---|
| 출처 데이터셋 | uspto-grants-2011_08 |
|---|
| ORD ID | ord-6bd2ac5a31464843987cb079c96df7b1 |
|---|
| 출처 메모 | uspto-grants-2011_08 |
|---|
