Thioctic Acid Impurity 38 synthesis
- Product Name:Thioctic Acid Impurity 38
- CAS Number:91009-30-2
- Molecular formula:C10H20O2S2
- Molecular Weight:236.39
Yield:91009-30-2 96%
Reaction Conditions:
Stage #1: Thioctic acidwith sodium tetrahydroborate;sodium hydroxide at 40; for 0.5 h;
Stage #2: methyl iodidewith sodium hydroxide at 20; for 0.75 h;
Steps:
1
EXAMPLE 1 Preparation of 6.8-to(benzylthio)octanoie acid dimethyl analogLipoic acid (I g, 0.000485 mol) was dissolved with stirring in 5 mL (1 equiv) of IM NaOH. Solid NaBH4 (0.183 g, 1 equiv) was added in one portion, and the resulting reaction mixture was heated to 40° C. After thirty minutes, the reaction solution had become completely colorless. 5 mL of 2M NaOH was then added, followed by 2 equivalents of methyl iodide (0.604 mL). The reaction solution was stirred at room temperature for 45 minutes. The reaction mixture was diluted with 10 mL of MTBE and acidified to pH <; 2 with concentrated HCl. The top organic layer was separated and concentrated on a rotary evaporator (rotovap). 6,8-dimethylthio-octanoic acid was isolated as a mobile oil, 1.1 g, 96%.
References:
WO2010/110771,2010,A2 Location in patent:Page/Page column 11
62-46-4
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