HCID 18374925, 화합물 → HCID 9877992, 화합물
반응식
[CH3:1][N:2]1[C:7]2[N:8]=[C:9](S(C)(=O)=O)[N:10]=[CH:11][C:6]=2[CH:5]=[CH:4][C:3]1=[O:16]>C(N)CCC>[CH2:3]([NH:2][C:9]1[N:10]=[CH:11][C:6]2[CH:5]=[CH:4][C:3](=[O:16])[N:2]([CH3:1])[C:7]=2[N:8]=1)[CH2:4][CH2:5][CH3:6]참가 물질
3
실험 절차
A solution of 8-methyl-2-methanesulfonyl-8H-pyrido[2,3-d]pyrimidin-7-one (200 mg, 0.83 mmol) in 2 mL of n-butylamine was stirred at room temperature for 10 minutes. The reaction mixture was partitioned between ethyl acetate and water, and the organic layer was washed with saturated sodium bicarbonate and brine, dried over magnesium sulfate, and concentrated in vacuo. A 4:1 mixture of hexane:ethyl acetate was added to the residue and the resultant solid collected by filtration to give 154 mg (79%) of 2-butylamino-8-methyl-8H-pyrido[2,3-d]pyrimidin-7-one, mp 146-147° C.
후처리
- customThe reaction mixture was partitioned between ethyl acetate and water
- washthe organic layer was washed with saturated sodium bicarbonate and brine
- dry with materialdried over magnesium sulfate
- concentrationconcentrated in vacuo
- additionA 4:1 mixture of hexane
- additionethyl acetate was added to the residue
- filtrationthe resultant solid collected by filtration
출처 및 근거
- ORD 기록
- ord-1af32eed8c99406daa91afaab1806f40
- 출처 데이터셋
- uspto-grants-2002_12
- 특허 번호
- US06498163B1
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