Water → [(R)-1-(6-chloro-1H-benzimidazol-2-yl)-2-methoxy-ethyl]-{2-[4-(4-chloro-phenyl)-piperazin-1-yl]-5-oxo-6,7-dihydro-5H-5lambda4-thieno[3,2-d]pyrimidin-4-yl}-amine

https://huagongshe.com/ja/reaction/70107

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	4-Chloro-2-[4-(4-chloro-phenyl)-piperazin-1-yl]-6,7-dihydro-thieno[3,2-d]pyrimidine 5-oxide	HCID 59475895	—
反応物	(1R)-1-(5-chloro-1H-benzimidazol-2-yl)-2-methoxyethylamine	HCID 59708426	—
溶媒	Dichloromethane	HCID 6344	—
溶媒	1,4-Dioxane	HCID 31275	—
生成物	[(R)-1-(6-chloro-1H-benzimidazol-2-yl)-2-methoxy-ethyl]-{2-[4-(4-chloro-phenyl)-piperazin-1-yl]-5-oxo-6,7-dihydro-5H-5lambda4-thieno[3,2-d]pyrimidin-4-yl}-amine	HCID 59708429	37.8%

反応条件

温度	120 °C

反応手順

200 mg 4-chloro-2-[4-(4-chloro-phenyl)-piperazin-1-yl]-6,7-dihydro-thieno[3,2-d]pyrimidine 5-oxide (cf Example 124), 235 mg (R)-1-(6-chloro-1H-benzimidazol-2-yl)-2-methoxy-ethylamine and 179.62 μl diisopropylethylamine are placed in 4 ml dioxane, and the mixture is heated to 120° C. in the microwave for 0.3 hours. Then the reaction mixture is combined with water and dichloromethane and extracted. The product is purified by semipreparative HPLC (method A). 113 mg of the product are obtained as a powder. Analytical HPLC-MS, (method B): RT=1.88 min.

情報源と証拠

DOI	10.6084/m9.figshare.5104873.v1
特許番号	US08822474B2
出典データセット	uspto-grants-2014_09
ORD ID	ord-d01a71046514423f8d801eb4965992b8
出典メモ	uspto-grants-2014_09