Thiocyanic acid, 3,3-dimethyl-2-oxobutyl ester synthesis
- Product Name:Thiocyanic acid, 3,3-dimethyl-2-oxobutyl ester
- CAS Number:57518-71-5
- Molecular formula:C7H11NOS
- Molecular Weight:157.23
13547-70-1
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Yield:57518-71-5 94%
Reaction Conditions:
in methanol at 55; for 2.5 h;
Steps:
[0795] Synthesis of intermediate (b)Into a reaction vessel, 120.5 g (1.48 mol) of sodium thiocyanate and 280 mL of methanol were introduced, and the internal temperature of the vessel was raised to 55°C. To this mixture, 200 g (1.48 mol) of (a) 1-chloropinacolone was dropped over 30 minutes. After finishing the dropping, the reaction was continued for 2 hours with the internal temperature of the vessel kept at 55°C. After finishing the reaction, the internal temperature of the vessel was reduced to 10°C, and 250 mL of water was added thereto. The mixture was then stirred at 10°C for 30 minutes. The crystal was then filtered and separated, thereby obtaining a white crystal of intermediate (b). The amount of the intermediate (b) was 218 g (yield 94%). Results of mass spectrometric analysis: (m/z) =158 ([M+l]+, 100%).
References:
WO2011/40628,2011,A1 Location in patent:Page/Page column 297
