Solvent-free micorowave-assisted multi-component reaction for preparation of 2-aminoketones as precursors of pseudoephedrine analogues
Li-Jian Ma; Tsutomu Inokuchi; Chem. Commun. 46 (2010) 7037–7039; doi:10.1039/c0cc00859a

data_7105626
_publ_section_title
;
 Solvent-free micorowave-assisted multi-component reaction for preparation
 of 2-aminoketones as precursors of pseudoephedrine analogues
;
_journal_issue                   37
_journal_name_full               'Chem. Commun.'
_journal_page_first              7037
_journal_page_last               7039
_journal_paper_doi               10.1039/c0cc00859a
_journal_volume                  46
_journal_year                    2010
_chemical_formula_moiety         'C18 H24 Br N O2 '
_chemical_formula_sum            'C18 H24 Br N O2'
_chemical_formula_weight         366.30
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                100.735(4)
_cell_angle_beta                 108.601(4)
_cell_angle_gamma                103.438(2)
_cell_formula_units_Z            2
_cell_length_a                   10.3812(5)
_cell_length_b                   11.6853(3)
_cell_length_c                   8.0564(5)
_cell_measurement_reflns_used    2469
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      25.3
_cell_measurement_theta_min      3.3
_cell_volume                     864.20(8)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_publication_material  'teXsan Ver. 1.11'
_computing_structure_refinement  'teXsan Ver. 1.10'
_computing_structure_solution    SIR97
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.9139
_diffrn_measured_fraction_theta_max 0.9139
_diffrn_measurement_device_type  'Rigaku RAXIS-IV Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.028
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            3384
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_exptl_absorpt_coefficient_mu    2.392
_exptl_absorpt_correction_T_max  0.550
_exptl_absorpt_correction_T_min  0.328
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Higashi, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_size_max          0.700
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.250
_refine_diff_density_max         0.98
_refine_diff_density_min         -0.64
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.542
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     199
_refine_ls_number_reflns         2737
_refine_ls_R_factor_gt           0.0696
_refine_ls_shift/su_max          0.0083
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00497|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1247
_reflns_number_gt                2461
_reflns_number_total             2889
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c0cc00859a.txt
_cod_data_source_block           ma
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C18 H24 Br N O2 '
_cod_database_code               7105626