Hydrochloric Acid → Ethyl 4-[(3-chloro-4-fluorophenyl)amino]-5,7-dihydro-6H-pyrrolo[3',4':4,5]thieno[2,3-d]pyrimidine-6-carboxylate

関与物質

役割	名称	HCID	仕込み量
反応物	Hydrochloric Acid	HCID 313	—
反応物	3-Chloro-4-fluoroaniline	HCID 9708	—
反応物	Ethyl12-chloro-7-thia-4,9,11-triazatricyclo[6.4.0.02,6]dodeca-1(8),2(6),9,11-tetraene-4-carboxylate	HCID 58116864	—
触媒	1,4-Dioxane	HCID 31275	—
溶媒	Isopropanol	HCID 3776	—
生成物	Ethyl 4-[(3-chloro-4-fluorophenyl)amino]-5,7-dihydro-6H-pyrrolo[3',4':4,5]thieno[2,3-d]pyrimidine-6-carboxylate	HCID 58116867	121.2%

反応条件

温度	80 °C

反応手順

Ethyl 4-chloro-5,7-dihydro-6H-pyrrolo[3′,4′:4,5]thieno[2,3-d]pyrimidine-6-carboxylate from Example 21A (250 mg, 0.88 mmol) was dissolved in 2-propanol (2 mL). 3-Chloro-4-fluoroanilin (135 mg, 0.93 mmol) and a 4 M solution of gaseous hydrogen chloride in dioxane (11 μL, 0.04 mmol) were added, and the mixture was heated to 80° C. overnight. The precipitate was collected by suction filtration to yield 419 mg of the crude product (70% purity, 83% yield), which was used in the next step without purification.

情報源と証拠

DOI	10.6084/m9.figshare.5104873.v1
特許番号	US08524722B2
出典データセット	uspto-grants-2013_09
ORD ID	ord-36e09b5a15964098b25b59eac5145b24
出典メモ	uspto-grants-2013_09