참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | Pyrimidine, 2,4-dichloro-5-methyl- | HCID 74508 | — |
| 반응물 | 2-(Propane-2-sulfonyl)aniline | HCID 12646366 | — |
| 용매 | N,N-dimethylformamide; methylsulfinylmethane | HCID 3013483 | — |
| 생성물 | 2-chloro-N-(2-(isopropylsulfonyl)phenyl)-5-methylpyrimidin-4-amine | HCID 59764473 | — |
반응 단계
To a suspension of 730 mg of NaH in a mixture of DMF/DMSO (25/2.5 ml) is added drop-wise at 0° C., 2.53 g (12.69 mmol) of 2-(iso-propylsulfonyl)benzenamine in DMF/DMSO (10 ml, ratio 9/1). The solution is stirred 30 minutes at 0° C. and 4.11 g (25.3 mmol, 2 eq.) of 2,4-dichloro-5-methylpyrimidine diluted in 10 ml of DMF/DMSO (ratio: 9/1) is added dropwise. The solution is warmed-up to room temperature and stirred overnight. After work-up, the crude product is directly crystallized from cold CH3CN in several batches to afford 2-chloro-N-(2-(iso-propylsulfonyl)phenyl)-5-methylpyrimidin-4-amine as pale creamy colored crystals: ESMS m/z 326.1 (M+H+).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08372858B2 |
|---|
| 출처 데이터셋 | uspto-grants-2013_02 |
|---|
| ORD ID | ord-9a70029a24c8438d9b3d1e1772fd6dc9 |
|---|
| 출처 메모 | uspto-grants-2013_02 |
|---|