참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium Carbonate | HCID 10340 | — |
| 반응물 | N-Cyclopropyl-N'-(4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)phenyl)urea | HCID 44119149 | — |
| 반응물 | HCID 89487530 | HCID 89487530 | — |
| 촉매 | Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+) | HCID 178418228 | — |
| 용매 | Water 1,2-dimethoxyethane | HCID 18180031 | — |
| 생성물 | HCID 71548238 | HCID 71548238 | — |
반응 단계
To a solution of 2-chloro-5,7-dihydro-4-((S)-3-methylmorpholino)thieno[3,4-d]pyrimidine (100 mg, 0.37 mmol) in DME/H2O (4:1, 10 mL) was added 1-cyclopropyl-3-(4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)phenyl)urea (124 mg, 0.41 mmol), and Na2CO3 (118 mg, 1.11 mmol) followed by addition of PdCl2(dppf) (15 mg, 0.02 mmol). The resulting mixture was heated to 70° C. and stirred overnight under nitrogen. The solvent was removed under reduced pressure to give a residue which was partitioned between ethyl acetate and water. The organic layer was washed with brine dried (Na2SO4) and concentrated to give a crude product which was purified by preparative TLC (DCM/MeOH=20/1) to give the desired product, as a yellow solid (20 mg, 13%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US09242993B2 |
|---|
| 출처 데이터셋 | uspto-grants-2016_01 |
|---|
| ORD ID | ord-27972c7b655c4253beb36f0f2e4230ad |
|---|
| 출처 메모 | uspto-grants-2016_01 |
|---|
