Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Trifluoroacetic acid methylene chloride → 1-[3-(4-Amino-7-piperidin-4-yl-7H-pyrrolo[2,3-d]pyrimidine-5-carbonyl)-phenyl]-3-(3,5-dichloro-phenyl)-urea
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Trifluoroacetic acid methylene chloride | HCID 21863450 | — |
| 반응물 | 4-(4-Amino-5-{3-[3-(3,5-dichloro-phenyl)-ureido]-benzoyl}-pyrrolo[2,3-d]pyrimidin-7-yl)-piperidine-1-carboxylic acid tert-butyl ester | HCID 67219160 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 1-[3-(4-Amino-7-piperidin-4-yl-7H-pyrrolo[2,3-d]pyrimidine-5-carbonyl)-phenyl]-3-(3,5-dichloro-phenyl)-urea | HCID 67219862 | 95.3% |
반응 단계
A solution of TFA/CH2Cl2 (0.49 mL/3.5 mL) was added to a solution of 4-(4-amino-5-{3-[3-(3,5-dichloro-phenyl)-ureido]-benzoyl}-pyrrolo[2,3-d]pyrimidin-7-yl)-piperidine-1-carboxylic acid tert-butyl ester (0.2 g, 0.32 mmol) in CH2Cl2 (1 mL) at 0 C. The reaction mixture was warmed to room temperature, stirred for 12 h, and concentrated in vacuo. The crude reaction mixture was quenched with H2O (5 mL) and Na2CO3 (5 mL) and extracted with CH2Cl2 (4×5 mL). The combined organic extracts were dried (MgSO4), filtered, and concentrated in vacuo to provide the title compound as a yellow solid (0.16 g, 93%). MS: 525.5 (MH+); HPLC Rf: 5.35 min. (HPLC method 4); HPLC purity: 84%.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07271262B2 |
| 출처 데이터셋 | uspto-grants-2007_09 |
| ORD ID | ord-d8ca7405ea6f4f99bbe217c03b7512c4 |
| 출처 메모 | uspto-grants-2007_09 |