Sodium Hydroxide → 5-Ethynyl-2,3-dimethoxypyridine

2,3-Dimethoxy-5-[(trimethylsilyl)ethynyl]pyridine (Intermediate 31) (9.8 g, 42 mmol) was dissolved in a mixture of aqueous sodium hydroxide (21 ml, 2 M, 42 mmol) and methanol (50 ml) to give a colourless solution which was stirred for 16 hours. The reaction was evaporated and the residue was partitioned between ethyl acetate and water before the organic layer was dried and concentrated in vacuo. The crude material was purified by (SiO2; 0-10% ethyl acetate in petrol) to afford 5-ethynyl-2,3-dimethoxypyridine (5.6 g, 82%).

1. customto give a colourless solution which
2. customThe reaction was evaporated
3. customthe residue was partitioned between ethyl acetate and water before the organic layer
4. customwas dried
5. concentrationconcentrated in vacuo
6. customThe crude material was purified by (SiO2; 0-10% ethyl acetate in petrol)

ORDレコード

ord-7a477c5919c743b684e780b8f7c73222

出典データセット

uspto-grants-2015_11

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09180122B2