Water → (R)-2-{2-[4-(4-CHLORO-PHENYL)-PIPERAZIN-1-YL]-5-OXO-6,7-DIHYDRO-5H-5lambda4-THIENO [3,2-D]PYRIMIDIN-4-YLAMINO}-4-METHYL-PENTAN-1-OL

https://huagongshe.com/ko/reaction/70103

참여 물질

역할	이름	HCID	투입량
반응물	Water	HCID 962	—
반응물	Diisopropylethylamine	HCID 81531	—
반응물	D(-)-Leucinol	HCID 2724002	—
반응물	4-Chloro-2-[4-(4-chloro-phenyl)-piperazin-1-yl]-6,7-dihydro-thieno[3,2-d]pyrimidine 5-oxide	HCID 59475895	—
용매	1,4-Dioxane	HCID 31275	—
생성물	(R)-2-{2-[4-(4-CHLORO-PHENYL)-PIPERAZIN-1-YL]-5-OXO-6,7-DIHYDRO-5H-5lambda4-THIENO [3,2-D]PYRIMIDIN-4-YLAMINO}-4-METHYL-PENTAN-1-OL	HCID 59708497	—

반응 조건

온도	120 °C

반응 단계

220 mg 4-chloro-2-[4-(4-chloro-phenyl)-piperazin-1-yl]-6,7-dihydro-thieno[3,2-d]pyrimidine 5-oxide (cf Example 124), 134.53 mg D-leucinol and 197.52 μl diisopropylethylamine are placed in 4 ml dioxane, heated to 120° C. in the microwave for 0.3 hours. Then the reaction mixture is mixed with water, the precipitate formed is suction filtered, washed and dried. The diastereomers are separated by preparative HPLC (method B). 43.9 mg of Diastereomer 1 (Example 53) and 46.9 mg of Diastereomer 2 (Example 69) are obtained as an oil. Analytical HPLC-MS (method B): Diastereomer 1, RT=1.86 min, Diastereomer 2, RT=1.90 min.

출처 및 근거

DOI	10.6084/m9.figshare.5104873.v1
특허 번호	US08822474B2
출처 데이터셋	uspto-grants-2014_09
ORD ID	ord-973ba9b476d042ecbe81c760274107eb
출처 메모	uspto-grants-2014_09