Triethylamine → 1-methyl-2-(6-methyl-[1,4]oxazepan-4-yl)-1H-[4,4']bipyrimidinyl-6-one

HRID 515455노트

반응식

HRID 515455 반응식
Cl[C:2]1[N:3]([CH3:15])[C:4](=[O:14])[CH:5]=[C:6]([C:8]2[CH:13]=[CH:12][N:11]=[CH:10][N:9]=2)[N:7]=1.Cl.[CH3:17][CH:18]1[CH2:24][O:23][CH2:22][CH2:21][NH:20][CH2:19]1.C(N(CC)CC)C>O1CCCC1>[CH3:15][N:3]1[C:4](=[O:14])[CH:5]=[C:6]([C:8]2[CH:13]=[CH:12][N:11]=[CH:10][N:9]=2)[N:7]=[C:2]1[N:20]1[CH2:19][CH:18]([CH3:17])[CH2:24][O:23][CH2:22][CH2:21]1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 179544602-Chloro-3-methyl-6-(pyrimidin-4-YL)pyrimidin-4-oneHCID 667185826-Methyl-1,4-oxazepane hydrochloride

생성물 1

HCID 667185661-methyl-2-(6-methyl-[1,4]oxazepan-4-yl)-1H-[4,4']bipyrimidinyl-6-one수율 60.3%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a slurry of 2-chloro-1-methyl-1H-[4,4′]bipyrimidinyl-6-one (113 mg, 0.507 mmol) and 6-methyl-[1,4]oxazepane hydrochloride (100 mg, 0.660 mmol) in tetrahydrofuran (1.1 mL) was added triethylamine (154 mg, 1.52 mmol) at room temperature. The mixture was stirred for 15 hours and partitioned between water and ethyl acetate. The organic layer was washed with brine, dried over sodium sulfate and concentrated in vacuo. The crude product was washed with ether and dried under reduced pressure to afford 1-methyl-2-(6-methyl-[1,4]oxazepan-4-yl)-1H-[4,4′]bipyrimidinyl-6-one (A087) as white solid (92.2 mg, 60%).

후처리

  1. custompartitioned between water and ethyl acetate
  2. washThe organic layer was washed with brine
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated in vacuo
  5. washThe crude product was washed with ether
  6. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-925f2806f00b4de08f9ad59fb23f2909
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09108957B2

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