Hydrochloride methanol → 1,4,5,6-Tetrahydro-N-methoxy-5-pyrimidinamine dihydrochloride
反応式
[ClH:1].[CH3:2][O:3][N:4]=[C:5]1[CH2:10][NH:9][CH:8]=[N:7][CH2:6]1.Cl.CO.[BH4-].CN(C)C>CO>[ClH:1].[ClH:1].[CH3:2][O:3][NH:4][CH:5]1[CH2:10][NH:9][CH:8]=[N:7][CH2:6]1参加物
5
実験手順
A solution of 1,6-dihydro-5-(4H)-pyrimidinone O-methyloxim monohydrochloride (2.8 g, 17.1 mmol) in dry methanol was added dropwise to a stirred solution of HCl/methanol (49 ml of a 3N solution) and trimethylamine borohydride (1.36 g, 18.7 mmol) at room temperature under a nitrogen atmosphere. After 1 hour the reaction product crystallised spontaneously. Recrystallization from methanol/ethyl acetate gave a light-brown material in 38% yield (1.30 g). Mp. 214.0° C.
後処理
- customAfter 1 hour the reaction product crystallised spontaneously
- customRecrystallization from methanol/ethyl acetate
- customgave a light-brown material in 38% yield (1.30 g)
出典と根拠
- ORDレコード
- ord-5d150106284f449cb8c5312a003774d5
- 出典データセット
- uspto-grants-1995_11
- 特許番号
- US05470856
反応ノート
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