(6-氯-2,3-二氢-1,4-苯并二恶英-2-基)甲醇

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

实验步骤: To (6-chloro-2,3-dihydrobenzo[1,4]dioxin-2-yl)methanol (9.5 mg, 0.042 mmol), PPh3 (17 mg, 0.066 mmol) and N-(t-butoxycarbonyl)sulfamide (16 mg, 0.083 mmol) in Ethyl acetate (0.5 mL) was added diisopropyl azodicarboxylate (DIAD, 0.013 mL, 0.066 mmol) dropwise. The resulting mixture was stirred at room temperature for 2 h (monitored with TLC 40% ethyl acetate-heptane and LC-MS) and then concentrated to a residue. The residue loaded onto a 12 g ISCO silica column in CH2Cl2 and eluted with 0-30% ethyl acetate/heptane to yield the title compound as a gum, which was used in the next step without further purification. concentrated to a residue eluted with 0-30% ethyl acetate/heptane

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

实验步骤: To (6-chloro-2,3-dihydrobenzo[1,4]dioxin-2-yl)methanol (9.5 mg, 0.042 mmol), PPh3 (17 mg, 0.066 mmol) and N-(t-butoxycarbonyl)sulfamide (16 mg, 0.083 mmol) in Ethyl acetate (0.5 mL) was added diisopropyl azodicarboxylate (DIAD, 0.013 mL, 0.066 mmol) dropwise. The resulting mixture was stirred at room temperature for 2 h (monitored with TLC 40% ethyl acetate-heptane and LC-MS) and then concentrated to a residue. The residue loaded onto a 12 g ISCO silica column in CH2Cl2 and eluted with 0-30% ethyl acetate/heptane to yield the title compound as a gum, which was used in the next step without further purification. concentrated to a residue eluted with 0-30% ethyl acetate/heptane