3-Methoxypropylamine → 4,6-Dichloro-N-(3-methoxypropyl)pyrimidin-2-amine
反応式
[CH3:1][O:2][CH2:3][CH2:4][CH2:5][NH2:6].Cl[C:8]1[N:13]=[C:12]([Cl:14])[CH:11]=[C:10]([Cl:15])[N:9]=1>O1CCCC1>[Cl:15][C:10]1[CH:11]=[C:12]([Cl:14])[N:13]=[C:8]([NH:6][CH2:5][CH2:4][CH2:3][O:2][CH3:1])[N:9]=1参加物
4
実験手順
48 g (0.54 mole) of 3-methoxypropylamine are added dropwise to 50 g (0.27 mole) of 2,4,6-trichloropyrimidine, dissolved in 300 ml of tetrahydrofuran, at -30° C. After the reaction mixture has thawed to room temperature and been stirred for a further six hours, it is poured into ice water and extracted with methylene chloride, the extract is dried over sodium sulphate and the solvent is removed. The resulting residue is subjected to steam distillation in the course of which 10.6 g (16.6% of theory) of the desired pyrimidine pass over as a solid, melting point 48° C.
後処理
- customhas thawed to room temperature
- extractionextracted with methylene chloride
- dry with materialthe extract is dried over sodium sulphate
- customthe solvent is removed
- distillationThe resulting residue is subjected to steam distillation in the course of which 10.6 g (16.6% of theory) of the desired pyrimidine pass over as a solid, melting point 48° C.
出典と根拠
- ORDレコード
- ord-2f1d646afc524ab9942ddc9a13be653d
- 出典データセット
- uspto-grants-1986_12
- 特許番号
- US04627872
反応ノート
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