Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Dimethylamine → 4-(3-Chloro-anilino)-6-(N,N-dimethyl-carbamoyl)-7H-pyrrolo[2,3-d]-pyrimidin
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Dimethylamine | HCID 674 | — |
| 반응물 | O-(2-Oxo-1(2H)-pyridyl)-N,N,N',N'-tetramethyluronium Tetrafluoroborate | HCID 2733204 | — |
| 반응물 | 6-carboxy-4-(3-chloroanilino)-7H-pyrrolo[2,3-d]pyrimidine | HCID 21262674 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 4-(3-Chloro-anilino)-6-(N,N-dimethyl-carbamoyl)-7H-pyrrolo[2,3-d]-pyrimidin | HCID 23282689 | — |
반응 단계
Under a N2 atmosphere, 97.6 mg (0.338 mmol) of 6-carboxy-4-(3-chloro-anilino)-7H-pyrrolo[2,3-d]pyrimidine are introduced into 7 ml of DMF, and 119 mg (0.40 mmol) of TPTU and a solution of 164 mg (33% in ethanol; 1.2 mmol) of dimethylamine in 1 ml of DMF are added thereto. After 2 hours, a further 30 mg of TPTU is added to the reaction solution, which is then stirred at RT for 2 days, then poured into 30 ml of ice-water, stirred, filtered and washed with water to yield the title compound; HPLC: tRet (Grad20)=9.5; TLC-Rf =0.38 (CH2Cl2 /methanol [10:1]); FAB-MS: (M+H)+ =316.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06140332 |
| 출처 데이터셋 | uspto-grants-2000_10 |
| ORD ID | ord-a81a4fed39b14dcf89dcd23eeae12b1a |
| 출처 메모 | uspto-grants-2000_10 |