α-氯代苯乙酸乙酯

反应条件: temp:-45.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 9.8 g of potassium tert-butylate were dissolved in 90 mL of DMF and cooled to −45° C. To this, a mixture of ethyl 2-chloro-2-phenylacetate (43.8 mmol, 8.7 g) and 1-fluoro-2-nitrobenzene (43.8 mmol, 4.6 mL) was gently added dropwise and stirring was continued for a further 20 minutes. The reaction mixture was set to pH 4 with aq. 16% strength. HCl, diluted with 25 mL of water, and extracted with EA (3×50 mL). Following combination of the organic phases, they were washed with water and sat. aq. NaCl solution, dried over MgSO4 and concentrated in vacuo. The resulting residue was purified by column chromatography (silica gel: mesh 100-200, eluent: 10% EA in cyclohexane) and yielded 5.9 g (44.9%) of the desired product. was gently added dropwise extracted with EA (3×50 mL) were washed with water and sat. aq. NaCl solution dried over MgSO4 concentrated in vacuo The resulting residue was purified by column chromatography (silica gel: mesh 100-200, eluent: 10% EA in cyclohexane)

反应条件: temp:-45.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 9.8 g of potassium tert-butylate were dissolved in 90 mL of DMF and cooled to −45° C. To this, a mixture of ethyl 2-chloro-2-phenylacetate (43.8 mmol, 8.7 g) and 1-fluoro-2-nitrobenzene (43.8 mmol, 4.6 mL) was gently added dropwise and stirring was continued for a further 20 minutes. The reaction mixture was set to pH 4 with aq. 16% strength. HCl, diluted with 25 mL of water, and extracted with EA (3×50 mL). Following combination of the organic phases, they were washed with water and sat. aq. NaCl solution, dried over MgSO4 and concentrated in vacuo. The resulting residue was purified by column chromatography (silica gel: mesh 100-200, eluent: 10% EA in cyclohexane) and yielded 5.9 g (44.9%) of the desired product. was gently added dropwise extracted with EA (3×50 mL) were washed with water and sat. aq. NaCl solution dried over MgSO4 concentrated in vacuo The resulting residue was purified by column chromatography (silica gel: mesh 100-200, eluent: 10% EA in cyclohexane)

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of triethylamine (63.5 mmol, 8.7 mL) in methanol there was added dropwise, at 0° C., α-chlorophenylacetyl chloride (53 mmol, 7.6 mL), and the reaction mixture was then stirred over a period of 3.5 h at room temperature. The reaction mixture was then added to 100 mL of water and extracted with EA (3×100 mL). Following the combination of the organic phases, they were dried over MgSO4 and concentrated in vacuo to give 8.76 g (83.4%) of product. extracted with EA (3×100 mL) were dried over MgSO4 concentrated in vacuo

反应条件: temp:-45.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 9.8 g of potassium tert. butylate were dissolved in 90 ml of DMF and cooled to −45° C. For this purpose, a mix of ethyl 2-chloro-2-phenylacetate (43.8 mmol, 8.7 g) and 1-fluoro-2-nitrobenzene (43.8 mmol, 4.6 ml) was carefully added dropwise and the mixture was stirred for a further 20 minutes. The reaction mix was set to pH 4 using 16% HCl, diluted with 25 ml of water and extracted with EE (3×50 ml). Once combined, the organic phases were washed with water and sat. aq. NaCl sol., dried over MgSO4 and concentrated under vacuum. The residue obtained was purified by column chromatography (silica gel: mesh 100-200, eluent: 10% EE in cyclohexane) and produced 5.9 g (44.9%) of product. was carefully added dropwise The reaction mix extracted with EE (3×50 ml) the organic phases were washed with water and sat. aq. NaCl sol. dried over MgSO4 concentrated under vacuum The residue obtained was purified by column chromatography (silica gel: mesh 100-200, eluent: 10% EE in cyclohexane)

反应条件: temp:-45.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 9.8 g of potassium tert. butylate were dissolved in 90 ml of DMF and cooled to −45° C. For this purpose, a mix of ethyl 2-chloro-2-phenylacetate (43.8 mmol, 8.7 g) and 1-fluoro-2-nitrobenzene (43.8 mmol, 4.6 ml) was carefully added dropwise and the mixture was stirred for a further 20 minutes. The reaction mix was set to pH 4 using 16% HCl, diluted with 25 ml of water and extracted with EE (3×50 ml). Once combined, the organic phases were washed with water and sat. aq. NaCl sol., dried over MgSO4 and concentrated under vacuum. The residue obtained was purified by column chromatography (silica gel: mesh 100-200, eluent: 10% EE in cyclohexane) and produced 5.9 g (44.9%) of product. was carefully added dropwise The reaction mix extracted with EE (3×50 ml) the organic phases were washed with water and sat. aq. NaCl sol. dried over MgSO4 concentrated under vacuum The residue obtained was purified by column chromatography (silica gel: mesh 100-200, eluent: 10% EE in cyclohexane)

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Chlorophenyl acetyl chloride (53 mmol, 7.6 ml) was added dropwise to a solution of triethylamine (63.5 mmol, 8.7 ml) in methanol at 0° C. and the mixture was subsequently stirred for 3.5 h at room temperature. The reaction mix was then placed in 100 ml of water and repeatedly extracted with EE (3×100 ml). Once combined, the organic phases were dried over MgSO4, concentrated under vacuum and 8.76 g (83.4%) of product was obtained. The reaction mix repeatedly extracted with EE (3×100 ml) the organic phases were dried over MgSO4 concentrated under vacuum

反应条件: temp:-45.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 9.8 g of potassium tert.butylate were dissolved in 90 ml of DMF and cooled to −45° C. For this purpose, a mix of ethyl 2-chloro-2-phenylacetate (43.8 mmol, 8.7 g) and 1-fluoro-2-nitrobenzene (43.8 mmol, 4.6 ml) was carefully added dropwise and the mixture was stirred for a further 20 minutes. The reaction mix was set to pH 4 using 16% HCl, diluted with 25 ml of water and extracted with EE (3×50 ml). Once combined, the organic phases were washed with water and sat. aq. NaCl sol., dried over MgSO4 and concentrated under vacuum. The residue obtained was purified by column chromatography (silica gel: mesh 100-200, eluent: 10% EE in cyclohexane) and produced 5.9 g (44.9%) of product. was carefully added dropwise The reaction mix extracted with EE (3×50 ml) the organic phases were washed with water and sat. aq. NaCl sol. dried over MgSO4 concentrated under vacuum The residue obtained was purified by column chromatography (silica gel: mesh 100-200, eluent: 10% EE in cyclohexane)

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Chlorophenyl acetyl chloride (53 mmol, 7.6 ml) was added dropwise to a solution of triethylamine (63.5 mmol, 8.7 ml) in methanol at 0° C. and the mixture was subsequently stirred for 3.5 h at room temperature. The reaction mix was then placed in 100 ml of water and repeatedly extracted with EE (3×100 ml). Once combined, the organic phases were dried over MgSO4, concentrated under vacuum and 8.76 g (83.4%) of product was obtained. The reaction mix repeatedly extracted with EE (3×100 ml) the organic phases were dried over MgSO4 concentrated under vacuum

反应条件: temp:-45.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 9.8 g of potassium tert.butylate were dissolved in 90 ml of DMF and cooled to −45° C. For this purpose, a mix of ethyl 2-chloro-2-phenylacetate (43.8 mmol, 8.7 g) and 1-fluoro-2-nitrobenzene (43.8 mmol, 4.6 ml) was carefully added dropwise and the mixture was stirred for a further 20 minutes. The reaction mix was set to pH 4 using 16% HCl, diluted with 25 ml of water and extracted with EtOAc (3×50 ml). Once combined, the organic phases were washed with water and sat. aq. NaCl sol., dried over MgSO4 and concentrated under vacuum. The resulting residue was purified by column chromatography (silica gel: mesh 100-200, eluent: 10% EtOAc in cyclohexane) and produced 5.9 g (44.9%) of product. was carefully added dropwise The reaction mix extracted with EtOAc (3×50 ml) the organic phases were washed with water and sat. aq. NaCl sol. dried over MgSO4 concentrated under vacuum The resulting residue was purified by column chromatography (silica gel: mesh 100-200, eluent: 10% EtOAc in cyclohexane)

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Chlorophenyl acetyl chloride (53 mmol, 7.6 ml) was added dropwise to a solution of triethylamine (63.5 mmol, 8.7 ml) in methanol at 0° C. and the mixture was subsequently stirred for 3.5 h at room temperature. The reaction mix was then placed in 100 ml of water and repeatedly extracted with EtOAc (3×100 ml). Once combined, the organic phases were dried over MgSO4, concentrated under vacuum and 8.76 g (83.4%) of product was obtained. The reaction mix repeatedly extracted with EtOAc (3×100 ml) the organic phases were dried over MgSO4 concentrated under vacuum

反应条件: temp:-45.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 9.8 g of potassium tert-butylate were dissolved in 90 mL of DMF and cooled to −45° C. To this, a mixture of ethyl 2-chloro-2-phenylacetate (43.8 mmol, 8.7 g) and 1-fluoro-2-nitrobenzene (43.8 mmol, 4.6 mL) was gently added dropwise and stirring was continued for a further 20 minutes. The reaction mixture was set to pH 4 with aq. 16% strength. HCl, diluted with 25 mL of water, and extracted with EA (3×50 mL). Following combination of the organic phases, they were washed with water and sat. aq. NaCl solution, dried over MgSO4 and concentrated in vacuo. The resulting residue was purified by column chromatography (silica gel: mesh 100-200, eluent: 10% EA in cyclohexane) and yielded 5.9 g (44.9%) of the desired product. was gently added dropwise extracted with EA (3×50 mL) were washed with water and sat. aq. NaCl solution dried over MgSO4 concentrated in vacuo The resulting residue was purified by column chromatography (silica gel: mesh 100-200, eluent: 10% EA in cyclohexane)

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of triethylamine (63.5 mmol, 8.7 mL) in methanol there was added dropwise, at 0° C., α-chlorophenylacetyl chloride (53 mmol, 7.6 mL), and the reaction mixture was then stirred over a period of 3.5 h at room temperature. The reaction mixture was then added to 100 mL of water and extracted with EA (3×100 mL). Following the combination of the organic phases, they were dried over MgSO4 and concentrated in vacuo to give 8.76 g (83.4%) of product. extracted with EA (3×100 mL) were dried over MgSO4 concentrated in vacuo