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CAS No. : | 1468-83-3 | MDL No. : | MFCD00005468 |
Formula : | C6H6OS | Boiling Point : | No data available |
Linear Structure Formula : | CH3C(O)C4H3S | InChI Key : | RNIDWJDZNNVFDY-UHFFFAOYSA-N |
M.W : | 126.18 | Pubchem ID : | 15116 |
Synonyms : |
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Signal Word: | Warning | Class: | |
Precautionary Statements: | P261-P280-P305+P351+P338 | UN#: | |
Hazard Statements: | H302-H315-H319-H332-H335 | Packing Group: | |
GHS Pictogram: |
* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
75% | Preparation 8 1-Thiophen-3-yl-ethylamine The synthetic procedure used in this preparation is outlined below in Scheme J. To a solution of 3-Acetylthiophene (2.0 g, 15.85 mmol) and ammonium acetate (12.2 g, 158.5 mmol) in methanol (50 mL) was added sodium cyanoborohydride (0.7 g, 11.1 mmol) in one portion. The reaction mixture was stirred overnight at room temperature. After removal of methanol, water (20 mL) was added to the residue and the resulting solution was basified by addition of sodium hydroxide to pH=13. The aqueous solution was extracted with dicholromethane and the combined organic phase was dried over sodium sulfate. Removal of the solvent under reduced pressure afforded 1.5 g 1-thiophen-3-yl-ethylamine, yield: 75%. MS (M+H)=128. | |
75% | Preparation 7: l-Thiophen-3-yl-ethylamine; The synthetic procedure used in this preparation is outlined below in Scheme I. To a solution of 3-Acetylthiophene (2.0 g, 15.85 mmol) and ammonium acetate (12.2 g, 158.5 mmol) in methanol (50 mL) was added sodium cyanoborohydride (0.7 g, 1 l.lmmol) in one portion. The reaction mixture was stirred overnight at RT. After removal of methanol, water (20 mL) was added to the residue and the resulting solution was basified by addition of sodium hydroxide to pH =13. The aqueous solution was ex- EPO <DP n="63"/>tracted with dichloromethane and the combined organic phase was dried over sodium sulfate. Removal of the solvent under reduced pressure afforded 1.5 g l-thiophen-3-yl- ethylamine, yield: 75%. MS (M+H) = 128. | |
75% | The synthetic procedure used in this preparation is outlined below in Scheme I. To a solution of 3-Acetylthiophene (2.0 g, 15.85 mmol) and ammonium acetate (12.2 g, 158.5 mmol) in methanol (50 mL) was added sodium cyanoborohydride (0.7 g, 11.1 mmol) in one portion. The reaction mixture was stirred overnight at room temperature. After removal of methanol, water (20 mL) was added to the residue and the resulting solution was basified by addition of sodium hydroxide to pH=13. The aqueous solution was extracted with dicholromethane and the combined organic phase was dried over sodium sulfate. Removal of the solvent under reduced pressure afforded 1.5 g 1-thiophen-3-yl-ethylamine, yield: 75%. MS (M+H)=128. |
75% | With ammonium acetate; sodium cyanoborohydride; In methanol; at 20.0℃; | Preparation 8 1-Thiophen-3-yl-ethylamine The synthetic procedure used in this preparation is outlined below in Scheme J. 3-Acetylthiophene (2.0 g, 15.85 mmol) and ammonium acetate (12.2 g, 158.5 mmol) in methanol (50 mL) was added sodium cyanoborohydride (0.7 g, 11.1 mmol) in one portion. The reaction mixture was stirred overnight at room temperature. After removal of methanol, water (20 mL) was added to the residue and the resulting solution was basified by addition of sodium hydroxide to pH=13. The aqueous solution was extracted with dichloromethane and the combined organic phase was dried over sodium sulfate. Removal of the solvent under reduced pressure afforded 1.5 g 1-thiophen-3-yl-ethylamine, yield: 75%. MS (M+H)=128. |
With ammonium acetate; sodium cyanoborohydride; In methanol; at 20.0℃; for 16.0h; | Step 1. To a solution of compound 3-1 (2 g, 15.9 mmol) in MeOH (20 mL) was added NH4OAc (12.2 g, 0.159 mol) and NaBH3CN (3.5 g, 55.5 mmol) at 20C. After the mixture was stirred at 20C for 16 h, it was concentrated. The residual was partitioned between EtOAc (50 mL) and NaOH solution (5 M, 5 mL) (adjust pH>13). The organic layer was washed with brine (20 mLx2), concentrated and purified by column (20 %-30 % MeOH in DCM) to give the crude compound 3-2 (800 mg, 40% yield). lH NMR (400 MHz, DMSO-/ ) delta 7.63 - 7.61 (d, J= 8.0 Hz, 1 H), 7.58 - 5.57 (m, 1 H), 7.25 - 7.23 (d, J= 8.0 Hz , 2 H), 4.53 - 4.48 (m, 1 H), 1.51 - 1.49 (d, J= 8.0 Hz , 3 H). |
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