反応 #1040238
関連文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US05278067
反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: The product of part (i) above (385 mg) in methanol (10 ml) was treated dropwise with thionyl chloride 0.4 ml, 5.5 mmol) at 0° C. and then the solution was stood at room temperature overnight. The excess methanol was removed by distillation at atmospheric pressure, and the residue was distilled to give the title compound (216 mg), [α]19 +33° (liquid, 1=0.1 dm, d22 =0.871), lit1 [α]23 +D D 32.2° (liquid 1=0.2 dm), υmax (CHBr3) 1725 cm-1 (ester), δ(CDCl3) 3.67 (s, 3H, CO2CH3), 2.57 (m, 1H, CH2CHCH2), 1.33 and 1.13 (m, 1H each, CH2CH3), 1.16 (d, J7 Hz, 3H, C--2H3), 0.89 (d, J7 Hz, 3H, C--4CH3), 0.87 (t, J7 Hz, 3H, CH2CH3) lit2 (NMR spectrum). The excess methanol was removed by distillation at atmospheric pressure the residue was distilled
ソース ID: ord-bc3178c0023644f78eaf3a880300df7c