4-甲基吗啉1,1-二氧化物

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 2-Chloroethyl chloroformate (0.72 ml, 6.7 mmol) was added dropwise to a solution of 4-methylthiomorpholine-1,1-dioxide (11.0 g, 6.7 mmol) in toluene (10 ml) at 0° C. under N2. After 10 min, the reaction was warmed and maintained at reflux for 2 h. On cooling, the reaction mixture was evaporated, partitioned between EtOAc and H2O, the organic layer separated and washed sequentially with dilute HCl and saturated brine, the organic layer dried over Na2SO4 and evaporated. The residue was taken up in MeOH (10 ml) and heated at reflux for 2 h, after which time the reaction mixture was evaporated and triturated with EtOAc to afford the subtitle compound (415 mg, 36%) as a solid. Rf 0.34 (CH2Cl2/MeOH/0.88NH3 90/10/1, v/v). MS m/z 136 (MH+). the reaction was warmed maintained at reflux for 2 h On cooling the reaction mixture was evaporated partitioned between EtOAc and H2O the organic layer separated washed sequentially with dilute HCl and saturated brine the organic layer dried over Na2SO4 evaporated heated at reflux for 2 h after which time the reaction mixture was evaporated triturated with EtOAc

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 2-Chloroethyl chloroformate (0.72 ml, 6.7 mmol) was added dropwise to a solution of 4-methylthiomorpholine-1,1-dioxide (1.0 g, 6.7 mmol) in toluene (10 ml) at 0° C. under N2. After 10 min, the reaction was warmed and maintained at reflux for 2 h. On cooling, the reaction mixture was evaporated and partitioned between EtOAc and H2O. The organic layer was separated and washed sequentially with dilute HCl and saturated brine, then dried over Na2SO4 and evaporated. The residue was taken up in MeOH (10 ml) and heated at reflux for 2 h, after which time the mixture was evaporated and triturated with EtOAc to afford the subtitle compound (415 mg, 36%) as a solid. Rf 0.34 (CH2Cl2/MeOH/0.88 NH3 90/10/1, v/v). MS m/z 136 (MH+). the reaction was warmed maintained at reflux for 2 h On cooling the reaction mixture was evaporated partitioned between EtOAc and H2O The organic layer was separated washed sequentially with dilute HCl and saturated brine dried over Na2SO4 evaporated heated at reflux for 2 h after which time the mixture was evaporated triturated with EtOAc

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 2-Chloroethyl chloroformate (0.72 ml, 6.7 mmol) was added dropwise to a solution of 4-methylthiomorpholine-1,1-dioxide (1.0 g, 6.7 mmol) in toluene (10 ml) at 0° C. under N2. After 10 min, the reaction was warmed and maintained at reflux for 2 h. On cooling, the reaction mixture was evaporated, partitioned between EtOAc and H2O, the organic layer separated and washed sequentially with dilute HCl and saturated brine, the organic layer dried over Na2SO4 and evaporated. The residue was taken up in MeOH (10 ml) and heated at reflux for 2 h, after which time the reaction mixture was evaporated and triturated with EtOAc to afford the subtitle compound (415 mg, 36%) as a solid. Rf 0.34 (CH2Cl2/MeOH/0.88NH3 90/10/1, v/v). MS m/z 136 (MH+). the reaction was warmed maintained at reflux for 2 h On cooling the reaction mixture was evaporated partitioned between EtOAc and H2O the organic layer separated washed sequentially with dilute HCl and saturated brine the organic layer dried over Na2SO4 evaporated heated at reflux for 2 h after which time the reaction mixture was evaporated triturated with EtOAc

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 2-Chloroethyl chloroformate (0.72 ml, 6.7 mmol) was added dropwise to a solution of 4-methylthiomorpholine-1,1-dioxide (1.0 g, 6.7 mmol) in toluene (10 ml) at 0° C. under N2. After 10 min, the reaction was warmed and maintained at reflux for 2 h. On cooling, the reaction mixture was evaporated, partitioned between EtOAc and H2O, the organic layer separated and washed sequentially with dilute HCl and saturated brine, the organic layer dried over Na2SO4 and evaporated. The residue was taken up in MeOH (10 ml) and heated at reflux for 2 h, after which time the reaction mixture was evaporated and triturated with EtOAc to afford the subtitle compound (415 mg, 36%) as a solid. Rf 0.34 (CH2Cl2/MeOH/0.88NH3 90/10/1, v/v). MS m/z 136 (MH+). the reaction was warmed maintained at reflux for 2 h On cooling the reaction mixture was evaporated partitioned between EtOAc and H2O the organic layer separated washed sequentially with dilute HCl and saturated brine the organic layer dried over Na2SO4 evaporated heated at reflux for 2 h after which time the reaction mixture was evaporated triturated with EtOAc

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 2-Chloroethyl chloroformate (0.72 ml, 6.7 mmol) was added dropwise to a solution of 4-methylthiomorpholine-1,1-dioxide (11.0 g, 6.7 mmol) in toluene (10 ml) at 0° C. under N2. After 10 min, the reaction was warmed and maintained at reflux for 2 h. On cooling, the reaction mixture was evaporated, partitioned between EtOAc and H2O, the organic layer separated and washed sequentially with dilute HCl and saturated brine, the organic layer dried over Na2SO4 and evaporated. The residue was taken up in MeOH (10 ml) and heated at reflux for 2 h, after which time the reaction mixture was evaporated and triturated with EtOAc to afford the subtitle compound (415 mg, 36%) as a solid. Rf 0.34 (CH2Cl2/MeOH/0.88NH3 90/10/1, v/v). MS m/z 136 (MH+). the reaction was warmed maintained at reflux for 2 h On cooling the reaction mixture was evaporated partitioned between EtOAc and H2O the organic layer separated washed sequentially with dilute HCl and saturated brine the organic layer dried over Na2SO4 evaporated heated at reflux for 2 h after which time the reaction mixture was evaporated triturated with EtOAc

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 2-Chioroethyl chloroformate (0.72 ml, 6.7 mmol) was added dropwise to a solution of 4-methylthiomorpholine-1,1-dioxide (1.0 g, 6.7 mmol) in toluene (10 ml) at 0C. under N2. After 10 min, the reaction was warmed and maintained at reflux for 2 h. On cooling, the reaction mixture was evaporated, partitioned between EtOAc and H2O, the organic layer separated and washed sequentially with dilute HCl and saturated brine, the organic layer dried over Na2SO4 and evaporated. The residue was taken up in MeOH (10 ml) and heated at reflux for 2 h, after which time the reaction mixture was evaporated and triturated with EtOAc to afford the subtitle compound (415 mg, 36%) as a solid. Rf 0.34 (CH2Cl2 /MeOH/0.88NH3 90/10/1, v/v). MS m/z 136 (MH+). the reaction was warmed maintained at reflux for 2 h On cooling the reaction mixture was evaporated partitioned between EtOAc and H2O the organic layer separated washed sequentially with dilute HCl and saturated brine the organic layer dried over Na2SO4 evaporated heated at reflux for 2 h after which time the reaction mixture was evaporated triturated with EtOAc

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 2-Chloroethyl chloroformate (0.72 ml, 6.7 mmol) was added dropwise to a solution of 4-methylthiomorpholine-1,1-dioxide (1.0 g, 6.7 mmol) in toluene (10 ml) at 0° C. under N2. After 10 min, the reaction was warmed and maintained at reflux for 2 h. On cooling, the reaction mixture was evaporated and partitioned between EtOAc and H2O. The organic layer was separated and washed sequentially with dilute HCl and saturated brine, then dried over Na2SO4 and evaporated. The residue was taken up in MeOH (10 ml) and heated at reflux for 2 h, after which time the mixture was evaporated and triturated with EtOAc to afford the subtitle compound (415 mg, 36%) as a solid. Rf 0.34 (CH2Cl2/MeOH/0.88 NH3 90/10/1, v/v). MS m/z 136 (MH+). the reaction was warmed maintained at reflux for 2 h On cooling the reaction mixture was evaporated partitioned between EtOAc and H2O The organic layer was separated washed sequentially with dilute HCl and saturated brine dried over Na2SO4 evaporated heated at reflux for 2 h after which time the mixture was evaporated triturated with EtOAc

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 2-Chloroethyl chloroformate (0.72 ml, 6.7 mmol) was added dropwise to a solution of 4-methylthiomorpholine-1,1-dioxide (1.0 g, 6.7 mmol) in toluene (10 ml) at 0° C. under N2. After 10 min, the reaction was warmed and maintained at reflux for 2 h. On cooling, the reaction mixture was evaporated, partitioned between EtOAc and H2O, the organic layer separated and washed sequentially with dilute HCl and saturated brine, the organic layer dried over Na2SO4 and evaporated. The residue was taken up in MeOH (10 ml) and heated at reflux for 2 h, after which time the reaction mixture was evaporated and triturated with EtOAc to afford the subtitle compound (415 mg, 36%) as a solid. Rf 0.34 (CH2Cl2/MeOH/0.88NH3 90/10/1, v/v). MS m/z 136 (MH+). the reaction was warmed maintained at reflux for 2 h On cooling the reaction mixture was evaporated partitioned between EtOAc and H2O the organic layer separated washed sequentially with dilute HCl and saturated brine the organic layer dried over Na2SO4 evaporated heated at reflux for 2 h after which time the reaction mixture was evaporated triturated with EtOAc

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 2-Chloroethyl chloroformate (0.72 ml, 6.7 mmol) was added dropwise to a solution of 4-methylthiomorpholine-1,1-dioxide (11.0 g, 6.7 mmol) in toluene (10 ml) at 0° C. under N2. After 10 min, the reaction was warmed and maintained at reflux for 2 h. On cooling, the reaction mixture was evaporated, partitioned between EtOAc and H2O, the organic layer separated and washed sequentially with dilute HCl and saturated brine, the organic layer dried over Na2SO4 and evaporated. The residue was taken up in MeOH (10 ml) and heated at reflux for 2 h, after which time the reaction mixture was evaporated and triturated with EtOAc to afford the subtitle compound (415 mg, 36%) as a solid. Rf 0.34 (CH2Cl2/MeOH/0.88NH3 90/10/1, v/v). MS m/z 136 (MH+). the reaction was warmed maintained at reflux for 2 h On cooling the reaction mixture was evaporated partitioned between EtOAc and H2O the organic layer separated washed sequentially with dilute HCl and saturated brine the organic layer dried over Na2SO4 evaporated heated at reflux for 2 h after which time the reaction mixture was evaporated triturated with EtOAc