乙基3-羟基-2,2-丙酸二甲酯

反应条件: temp:0.00; pressure:0.00; stir:

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

实验步骤: To a stirred solution of ethyl 3-hydroxy-2,2-dimethylpropanoate (3.0 g, 20.52 mmol) in DMF (15 mL) was added DBU (3.10 g, 20.52 mmol) at RT followed by slow addition of CS2 (3.12 g, 41.0 mmol) over a period of 10 minutes. The reaction mixture was stirred at RT for 30 min, and then cooled to 10° C. prior to addition of MeI (6.58 mL, 103 mmol). The reaction mixture was stirred for 2 h at RT after which it was quenched with ice water and extracted with diethyl ether (2×25 mL). The combined organic layer was dried over Na2SO4, filtered and the filtrate evaporated to afford Intermediate 212A as a pale yellow liquid (3.0 g, 62%). 1H NMR (300 MHz, chloroform-d) δ ppm 4.59 (s, 2H), 4.19 (q, J=7.05 Hz, 2H), 2.55 (s, 3H), 1.23-1.29 (m, 9H). cooled to 10° C. The reaction mixture was stirred for 2 h at RT after which it was quenched with ice water extracted with diethyl ether (2×25 mL) The combined organic layer was dried over Na2SO4 filtered the filtrate evaporated

反应条件: temp:0.00; pressure:0.00; stir:

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

实验步骤: The title compound was prepared following the procedure described in Intermediate 68 using 2,2-dimethyl-3-hydroxypropionic acid ethyl ester and benzyl chloride.

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

实验步骤: To a solution of 2,2-dimethyl-3-hydroxypropionic acid ethyl ester (1.3 g, 10.0 mmol) in CH3CN (30 mL) was added Ag2O (11.5 g, 50.0 mmol) and methyl iodide (0.56 mL, 11 mmol). The reaction mixture was stirred at rt for 12 h and quenched with a saturated aqueous NH4Cl. The mixture was filtered though Celite, the filtrate concentrated in vacuo, and the residue was purified by column chromatography (EtOAc/Hex=1/10) to give the title compound (1.34 g, 91.2%). quenched with a saturated aqueous NH4Cl The mixture was filtered though Celite the filtrate concentrated in vacuo the residue was purified by column chromatography (EtOAc/Hex=1/10)

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

实验步骤: To a stirred solution of ethyl 3-hydroxy-2,2-dimethylpropanoate (3.0 g, 20.52 mmol) in DMF (15 mL) was added DBU (3.10 g, 20.52 mmol) at RT followed by slow addition of CS2 (3.12 g, 41.0 mmol) over a period of 10 minutes. The reaction mixture was stirred at RT for 30 min, and then cooled to 10° C. prior to addition of MeI (6.58 mL, 103 mmol). The reaction mixture was stirred for 2 h at RT after which it was quenched with ice water and extracted with diethyl ether (2×25 mL). The combined organic layer was dried over Na2SO4, filtered and the filtrate evaporated to afford Intermediate 212A as a pale yellow liquid (3.0 g, 62%). 1H NMR (300 MHz, chloroform-d) δ ppm 4.59 (s, 2H), 4.19 (q, J=7.05 Hz, 2H), 2.55 (s, 3H), 1.23-1.29 (m, 9H). cooled to 10° C. The reaction mixture was stirred for 2 h at RT after which it was quenched with ice water extracted with diethyl ether (2×25 mL) The combined organic layer was dried over Na2SO4 filtered the filtrate evaporated