4-Aminopyridine catalyzed direct and regioselective acylation of N-tosylhydrazide.
Namba, Kosuke; Shoji, Isamu; Nishizawa, Mugio; Tanino, Keiji; Organic letters 11 (2009) 4970–4973; doi:10.1021/ol9021194

data_1504251
_publ_section_title
;
 4-Aminopyridine catalyzed direct and regioselective acylation of
 N-tosylhydrazide.
;
_journal_issue                   21
_journal_name_full               'Organic letters'
_journal_page_first              4970
_journal_page_last               4973
_journal_paper_doi               10.1021/ol9021194
_journal_volume                  11
_journal_year                    2009
_chemical_formula_moiety         'C13 H20 N2 O3 S '
_chemical_formula_sum            'C13 H20 N2 O3 S'
_chemical_formula_weight         284.37
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 85.983(11)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            8
_cell_length_a                   22.641(4)
_cell_length_b                   5.6658(16)
_cell_length_c                   22.789(6)
_cell_measurement_reflns_used    10562
_cell_measurement_temperature    123.1
_cell_measurement_theta_max      27.3
_cell_measurement_theta_min      3.6
_cell_volume                     2916.2(12)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SIR92
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.179
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            22745
_diffrn_reflns_theta_full        27.27
_diffrn_reflns_theta_max         27.27
_exptl_absorpt_coefficient_mu    0.228
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.310
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1216.00
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.64
_refine_diff_density_min         -3.61
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.801
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     395
_refine_ls_number_reflns         22745
_refine_ls_R_factor_gt           0.1074
_refine_ls_shift/su_max          0.0370
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0005Fo^2^ + 2.0000\s(Fo^2^) + 0.5000]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1751
_reflns_number_gt                9161
_reflns_number_total             6463
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ol9021194_si_002.cif
_cod_data_source_block           '_090907___________________'
_cod_original_cell_volume        2916.1(13)
_cod_original_formula_sum        'C13 H20 N2 O3 S '
_cod_database_code               1504251