Tetrahydrofuran → N-{4-[2-(4-cyclopropylpiperazin-1-yl)benzothiazol-6-yl]phenyl}-acetamide

温度

60 °C

To a solution of 6-bromo-2-(4-cyclopropylpiperazin-1-yl)benzothiazole (500 mg, 1.48 mmol) and 4-acetamidophenylboronic acid (319 mg, 1.78 mmol) in a 5:1 mixture of THF and H2O (20 mL) was added Pd2(dba)3 (240 mg, 0.148 mmol), followed by P(t-Bu)3BF4 (86 mg, 0.296 mmol) and K3PO4.H2O (1.97 g, 7.4 mmol). The mixture was heated at 60° C. for 3 h, filtered and the volatiles were evaporated. Water (5 mL) was added and the mixture was extracted with CH2Cl2 (3×20 mL). The combined organic extracts were dried (Na2SO4) and concentrated. The residue was purified by the preparative HPLC to give 42 mg (7%) of N-{4-[2-(4-cyclopropylpiperazin-1-yl)benzothiazol-6-yl]phenyl}-acetamide as a trifluoroacetate salt.

1. filtrationfiltered
2. customthe volatiles were evaporated
3. additionWater (5 mL) was added
4. extractionthe mixture was extracted with CH2Cl2 (3×20 mL)
5. dry with materialThe combined organic extracts were dried (Na2SO4)
6. concentrationconcentrated
7. customThe residue was purified by the preparative HPLC

ORDレコード

ord-004eeb9ecaf449119425dff3259cc876

出典データセット

uspto-grants-2014_07

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08772285B2