iptakalim synthesis
- Product Name:iptakalim
- CAS Number:642407-44-1
- Molecular formula:C9H21N
- Molecular Weight:143.27
Yield:642407-44-1 80%
Reaction Conditions:
in hexane at 0;
Steps:
1.3
Method 3. a solution of 0.10mole enamine (prepared from the condensation of methyl iso-propyl ketone and iso-propylamine) in 20mL hexane was filled with N2 and added dropwise to a solution containing 0.10 mole lithium methide with stirring in ice bath. After the reaction is complete, the mixture was poured into 500g glacial water, and stirred. The aqueous layer was extracted with ether (×2). The resulting organic layer was concentrated. 3N hydrochloric acid was added to acified the organic layer to pH<1. The mixture was kept for ten minutes and adjusted to pH>11 with 10% aqueous sodium hydroxide, then extracted with ether (×3). The extract was dried over anhydrous potassium carbonate and filtered. The filtrate was distilled at atmosphere to give a fraction of bp 140-145°C with a yield of 80%.
References:
EP1386908,2004,A1 Location in patent:Page 20-21
