Solvent-controlled two-step one-pot syntheses of α-X (X = Br or Cl) enamino ketones/esters and 3-(2,5-dioxopyrrolidin-1-yl)acrylate by using terminal carbonyl alkynes.
Chen, Xiao Yun; Yuan, Shuxia; Chen, Yan; Sun, Chenyang; Tang, Yaonan; Chen, Guang; Zhu, Baocheng; Chen, Kaiwei; Zheng, Shaojun; Cheng, Xiaofang; Organic & biomolecular chemistry 19 (2021) 7914–7919; doi:10.1039/d1ob01308d

data_7158264
_publ_section_title
;
 Solvent-controlled two-step one-pot syntheses of \a-X (X = Br or Cl)
 enamino ketones/esters and 3-(2,5-dioxopyrrolidin-1-yl)acrylate by using
 terminal carbonyl alkynes.
;
_journal_issue                   36
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              7914
_journal_page_last               7919
_journal_paper_doi               10.1039/d1ob01308d
_journal_volume                  19
_journal_year                    2021
_chemical_formula_sum            'C9 H14 Br N O3'
_chemical_formula_weight         264.12
_space_group_crystal_system      triclinic
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_audit_update_record
;
2021-07-04 deposited with the CCDC.	2021-08-24 downloaded from the CCDC.
;
_cell_angle_alpha                109.638(4)
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_cell_angle_gamma                101.081(5)
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_cell_volume                     544.76(6)
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      296(2)
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_diffrn_measured_fraction_theta_max 0.974
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.974
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_diffrn_reflns_theta_max         27.657
_diffrn_reflns_theta_min         3.163
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_refine_diff_density_max         0.802
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         2473
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
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_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0610P)^2^+0.0633P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0907
_refine_ls_wR_factor_ref         0.0953
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2016
_reflns_number_total             2473
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ob01308d2.cif
_cod_data_source_block           1
_cod_depositor_comments          'Adding full bibliography for 7158264.cif.'
_cod_database_code               7158264
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.419
_shelx_estimated_absorpt_t_max   0.520
_shelx_res_checksum              92588
_shelx_hkl_checksum              91209