HCID 18374925, 화합물 → HCID 9877992, 화합물

HRID 2300064노트

반응식

HRID 2300064 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

  1. customThe reaction mixture was partitioned between ethyl acetate and water
  2. washthe organic layer was washed with saturated sodium bicarbonate and brine
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated in vacuo
  5. additionA 4:1 mixture of hexane
  6. additionethyl acetate was added to the residue
  7. filtrationthe resultant solid collected by filtration

출처 및 근거

ORD 기록
ord-1af32eed8c99406daa91afaab1806f40
출처 데이터셋
uspto-grants-2002_12
특허 번호
US06498163B1

반응 노트

불러오는 중…