2-Bromopyrimidine → (R)-2-(3-methylpiperazin-1-yl)pyrimidine
反応式
[CH3:1][C@@H:2]1[CH2:7][NH:6][CH2:5][CH2:4][NH:3]1.Br[C:9]1[N:14]=[CH:13][CH:12]=[CH:11][N:10]=1>C1(C)C(C)=CC=CC=1>[CH3:1][C@H:2]1[NH:3][CH2:4][CH2:5][N:6]([C:9]2[N:14]=[CH:13][CH:12]=[CH:11][N:10]=2)[CH2:7]1参加物
4
実験手順
To a solution of (R)-2-methyl piperazine (4.0 g, 40 mmol) in xylene (100 mL) at 140° C. under nitrogen was added 2-bromo pyrimidine (6.36 g, 40 mmol) slowly over a period of 30 min. The heating was continued for additional 15 h and cooled. The solid precipitate was filtered and dried under suction and neutralized with a saturated aqueous solution of sodium bicarbonate. The product was extracted with DCM (2×50 mL), dried and evaporated to afford the title compound as a liquid (2.4 g, 34%). TLC—Chloroform/MeOH (8/2); Rf: 0.2.
後処理
- temperaturecooled
- filtrationThe solid precipitate was filtered
- customdried under suction
- extractionThe product was extracted with DCM (2×50 mL)
- customdried
- customevaporated
出典と根拠
- ORDレコード
- ord-aebcd8b8593343bfba60394dea781607
- 出典データセット
- uspto-grants-2011_08
- 特許番号
- US08008302B2
反応ノート
読み込み中…