(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_7112573
_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            'C22 H19 I N2 O2'
_chemical_formula_weight         470.05
_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                 94.331(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.3912(4)
_cell_length_b                   12.3586(6)
_cell_length_c                   20.4375(10)
_cell_measurement_temperature    296(2)
_cell_volume                     1861.53(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0238
_diffrn_reflns_av_sigmaI/netI    0.0203
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            15729
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.59
_exptl_absorpt_coefficient_mu    1.742
_exptl_crystal_density_diffrn    1.682
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             936
_refine_diff_density_max         0.614
_refine_diff_density_min         -0.736
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.834
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         4043
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.834
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_gt           0.0242
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.3005P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0906
_refine_ls_wR_factor_ref         0.1041
_reflns_number_gt                3497
_reflns_number_total             4043
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2md00273f.txt
_cod_data_source_block           ils_drl_03_1
_cod_database_code               7112573