Methylamine → HCID 19756475、化合物
反応式
Br[CH2:2][CH2:3][C:4]1[CH:5]=[CH:6][C:7]2[O:11][CH2:10][CH2:9][C:8]=2[CH:12]=1.[CH3:13][NH2:14]>CO>[O:11]1[C:7]2[CH:6]=[CH:5][C:4]([CH2:3][CH2:2][NH:14][CH3:13])=[CH:12][C:8]=2[CH2:9][CH2:10]1参加物
4
実験手順
A solution of 5-(2-bromoethyl)-2,3-dihydrobenzofuran (1.5 g-see Preparation 20) in 33% methylamine in methanol (40 ml) was heated at 100° C. in a stainless steel pressure vessel for 6 hours then concentrated in vacuo. The residue was partitioned between dichloromethane (50 ml) and 10% aqueous sodium carbonate (50 ml). The layers were separated and the aqueous layer was further extracted with dichloromethane (2×50 ml). The aqueous layer was concentrated in vacuo to give a solid which was triturated with boiling 2-propanol. The mixture was filtered and the filtrate concentrated in vacuo to give a solid which was purified by column chromatography on silica eluting with dichloromethane containing methanol (0% up to 1%). The product-containing fractions were combined and concentrated in vacuo to give the title compound as a colourless solid, yield, 0.31 g, m.p. 153°-155° C.