Hydrochloric Acid → HCID 14231025, compound
Reaction equation
C(=[N:8][CH2:9][C:10]#[C:11][C:12]1[S:13][CH:14]=[CH:15][CH:16]=1)C1C=CC=CC=1.Cl>O>[S:13]1[CH:14]=[CH:15][CH:16]=[C:12]1[C:11]#[C:10][CH2:9][NH2:8]Participants
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 60 °C
Procedure
To 17.7 g of this toluene solution, 36% hydrochloric acid (1.27 g, 12.5 mol) was added dropwise at 60° C. over 10 minutes, followed by stirring at 60° C. for 1.5 hours. Then, 4 g of water was added and the mixed solution was separated to obtain the aqueous phase and organic phase. The organic phase was extracted once with 2.5 g of water and the resulting aqueous phase was combined with the above aqueous phase. To this aqueous phase, 15 g of toluene was added and an aqueous 27% sodium hydroxide solution was added dropwise at 23° C. over 15 minutes, followed by stirring at 23° C. for 0.5 hours. After separating at the same temperature, the resulting organic phase was washed with 5 g of an aqueous saturated sodium chloride solution, concentrated and dried to obtain 3-(2-thienyl)-2-propynylamine (0.73 g, purity: 87%, yield: 77%).
Workup
- customthe mixed solution was separated
- customto obtain the aqueous phase and organic phase
- extractionThe organic phase was extracted once with 2.5 g of water
- additionTo this aqueous phase, 15 g of toluene was added
- additionan aqueous 27% sodium hydroxide solution was added dropwise at 23° C. over 15 minutes
- stirringby stirring at 23° C. for 0.5 hours
- customAfter separating at the same temperature
- washthe resulting organic phase was washed with 5 g of an aqueous saturated sodium chloride solution
- concentrationconcentrated
- customdried
Sources & evidence
- ORD record
- ord-ba8b5033d3674b738d2d8fff5bc66973
- Source dataset
- uspto-grants-1998_05
- Patent number
- US05756769
Reaction notes
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