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

HRID 515455ノート

反応式

HRID 515455 の反応式
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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-925f2806f00b4de08f9ad59fb23f2909
出典データセット
uspto-grants-2015_08
特許番号
US09108957B2

反応ノート

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