Water → 2-[[2-Amino-5-[[(2,3-difluorophenyl)methyl]thio]thiazolo[4,5-d]pyrimidin-7-yl]amino]-2-methyl-1,3-propanediol

関与物質

役割	名称	HCID	仕込み量
反応物	Water	HCID 962	—
反応物	Diisopropylethylamine	HCID 81531	—
反応物	2-Amino-2-methylpropane-1,1-diol	HCID 5244174	—
反応物	7-Chloro-5-[[(2,3-difluorophenyl)methyl]thio]-thiazolo[4,5-d]pyrimidin-2-amine	HCID 11221650	—
溶媒	N-methyl-2-pyrrolidone	HCID 13387	—
生成物	2-[[2-Amino-5-[[(2,3-difluorophenyl)methyl]thio]thiazolo[4,5-d]pyrimidin-7-yl]amino]-2-methyl-1,3-propanediol	HCID 22649035	42%

反応条件

温度	110 °C

反応手順

The product from step (d) (1.5 g) was suspended in NMP (10 ml), then Hunigs base (1.5 ml) and 2-Amino-2-methylpropanediol (1.37 g) added. Reaction mixture heated to 110° C. under N2 for 4 hrs. A further aliquot of 2-Amino-2-methylpropanediol (0.685 g) was added and mixture heated at 110° C. for 5 hrs. Mixture poured in to water (400 ml) and solid was collected by filtration. Purified by column chromatography (EtOAc: Methanol (95:5)) to give 0.756 g of product. 42% yield.

情報源と証拠

DOI	10.6084/m9.figshare.5104873.v1
特許番号	US07585867B2
出典データセット	uspto-grants-2009_09
ORD ID	ord-5e06f1e3b0214ea78b27093ecf157865
出典メモ	uspto-grants-2009_09