2-Vinylpyridine → HCID 86660912, compound
Reaction equation
[C:1]([OH:4])(=[S:3])[CH3:2].[CH:5]([C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][N:8]=1)=[CH2:6]>>[C:1]([O:4][CH2:6][CH2:5][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][N:8]=1)(=[S:3])[CH3:2]Participants
Conditions
- Temperature
- 5 °C
Procedure
Into a 100-mL four-necked flask equipped with a nitrogen gas introduction tube, thermometer, Dimroth condenser, and dropping funnel was introduced 15.22 g (0.20 mol) of thioacetic acid (manufactured by Tokyo Kasei Kogyo Co., Ltd.). The contents began to be stirred, and nitrogen was introduced. Thereafter, the contents were cooled to 5° C. or lower with an ice bath, and 21.03 g (0.20 mol) of 2-vinylpyridine was added dropwise thereto through the dropping funnel over 1 hour. After completion of the dropwise addition, the ice bath was removed, and the mixture was stirred at room temperature for further 1 hour and reacted. After completion of the reaction, the liquid reaction mixture was subjected to vacuum distillation under the conditions of a bath temperature of 120° C. and a pressure of 0.8 kPa to obtain 27.8 g of 2-pyridylethyl thioacetate. As a result of analysis by gas chromatography, the 2-pyridylethyl thioacetate was found to have a purity of 96.8% and the yield thereof was found to be 78.2%.
Workup
- customInto a 100-mL four-necked flask equipped with a nitrogen gas introduction tube
- additionnitrogen was introduced
- additionAfter completion of the dropwise addition
- customthe ice bath was removed
- stirringthe mixture was stirred at room temperature for further 1 hour
- customreacted
- customAfter completion of the reaction
- customthe liquid reaction mixture
- distillationwas subjected to vacuum distillation under the conditions of a bath temperature of 120° C.
Sources & evidence
- ORD record
- ord-51572c5f6e6646c2b35c28a36fc16f6b
- Source dataset
- uspto-grants-2013_05
- Patent number
- US08445731B2
Reaction notes
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