(Pd/C-mediated)coupling‒iodocyclization‒coupling strategy in discovery of novel PDE4 inhibitors: a new synthesis of pyrazolopyrimidines
Mahesh Kumar, P.; Siva Kumar, K.; Meda, Chandana L. T.; Rajeshwar Reddy, G.; Mohakhud, Pradeep K.; Mukkanti, K.; Rama Krishna, G.; Malla Reddy, C.; Rambabu, D.; Shiva Kumar, K.; Krishna Priya, K.; Chennubhotla, Keerthana Sarma; Banote, Rakesh Kumar; Kulkarni, Pushkar; Parsa, Kishore V. L.; Pal, Manojit; MedChemComm 3 (2012) 667–; doi:10.1039/c2md00273f

data_7112572
_publ_section_title
;
 (Pd/C-mediated)coupling--iodocyclization--coupling strategy in discovery
 of novel PDE4 inhibitors: a new synthesis of pyrazolopyrimidines
;
_journal_issue                   6
_journal_name_full               MedChemComm
_journal_page_first              667
_journal_paper_doi               10.1039/c2md00273f
_journal_volume                  3
_journal_year                    2012
_chemical_formula_sum            'C28 H28 N2 O2'
_chemical_formula_weight         436.22
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 115.645(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.2480(13)
_cell_length_b                   12.5719(10)
_cell_length_c                   14.0243(12)
_cell_measurement_temperature    296(2)
_cell_volume                     2423.6(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_av_sigmaI/netI    0.0349
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            14662
_diffrn_reflns_theta_full        22.94
_diffrn_reflns_theta_max         22.94
_diffrn_reflns_theta_min         2.91
_exptl_absorpt_coefficient_mu    0.076
_exptl_crystal_density_diffrn    1.191
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             916
_refine_diff_density_max         0.726
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.591
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         3278
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.591
_refine_ls_R_factor_all          0.1569
_refine_ls_R_factor_gt           0.1304
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.1739P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3633
_refine_ls_wR_factor_ref         0.3845
_reflns_number_gt                2433
_reflns_number_total             3278
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2md00273f.txt
_cod_data_source_block           ils_drl_07_1
_cod_database_code               7112572