5-Chloro-2-furaldehyde → 10-(5-Chlorofuran-2-yl)-5-(3-chlorophenyl)-1,3-dimethyl-7,8,9,10-tetrahydropyrazino[1',2':1,2]pyrrolo[3,4-d]pyrimidine-2,4(1H,3H)-dione

温度

50 °C

6-(2-Amino-ethyl)-5-(3-chloro-phenyl)-1,3-dimethyl-1,6-dihydro-pyrrolo[3,4-d]pyrimidine-2,4-dione (Intermediate B) (150 mg, 0.451 mmol) and 5-chlorofuran-2-carbaldehyde (commercially available, 58.8 mg, 0.451 mmol) were suspended in ethanol (1.2 ml). The mixture was heated at 50° C. under microwave irradiation for 1 hour. TFA (4 drops) was added to the reaction mixture and heating continued at 60° C. for a further 30 mins under microwave irradiation. The reaction mixture was diluted with ethanol (0.5 mL) and purified using mass directed HPLC. The product containing fractions were combined and evaporated under reduced pressure to afford a white solid which was dried under vacuum at 50° C. for 16 h to afford the title compound as a pale tan solid;

1. temperatureheating
2. customcontinued at 60° C. for a further 30 mins under microwave irradiation
3. custompurified
4. additionThe product containing fractions
5. customevaporated under reduced pressure
6. customto afford a white solid which
7. customwas dried under vacuum at 50° C. for 16 h

ORDレコード

ord-5a51311e7c1f464badbed1b4e2494218

出典データセット

uspto-grants-2016_04

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09303035B2