2,2,2-tribromoethanol

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Tribromoethanol (43.8 parts) was converted to the corresponding chloroformate by reaction with 40 parts of phosgene in the presence of a stoichiometric amount of base. The purified intermediate was reacted with an excess of sodium azide to produce the β,β,β-tribromoethyl azidoformate.

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Tribromoethanol (43.8 parts) was converted to the corresponding chloroformate by reaction with 40 parts of phosgene in the presence of a stoichiometric amount of base. The purified intermediate was reacted with an excess of sodium azide to produce the β,β,β-tribromoethyl azidoformate.

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Tribromoethanol (43.8 parts) was converted to the corresponding chloroformate by reaction with 40 parts of phosgene in the presence of a stoichiometric amount of base. The purified intermediate was reacted with an excess of sodium azide to produce the β,β,β-tribromoethyl azidoformate.

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Tribromoethanol (43.8 parts) was converted to the corresponding chloroformate by reaction with 40 parts of phosgene in the presence of a stoichiometric amount of base. The purified intermediate was reacted with an excess of sodium azide to produce the β,β,β-tribromoethyl azidoformate.

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A first solution comprising tribromoethanol (50 g, 177 mmol) and triethylamine (19.73 g, 195 mmol) dissolved in 70 g of diethylether was prepared. A second solution comprising methacryloyl chloride (20.39 g, 195 mmol) dissolved in 70 g of diethylether was added dropwise to the first solution followed by stirring for four hours at room temperature. The resulting solution was then added to water, and the organic phase was extracted. The organic phase was distilled to yield 32.85 g of TBEMA (52.9% yield). was prepared was added dropwise to the first solution the organic phase was extracted The organic phase was distilled to yield 32.85 g of TBEMA (52.9% yield)

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A first solution including tribromoethanol (50 g, 177 mmol) and triethylamine (19.73 g, 195 mmol) dissolved in 50 g of diethylether was prepared. A second solution comprising acryloyl chloride (17.65 g, 195 mmol) dissolved in 50 g of diethylether was added dropwise to the first solution followed by stirring for four hours at room temperature. The resulting solution was then added to water, and the organic phase was extracted. The organic phase was distilled to yield 48.38 g of TBEA (72.5% yield). was prepared was added dropwise to the first solution the organic phase was extracted The organic phase was distilled to yield 48.38 g of TBEA (72.5% yield)

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A first solution including tribromoethanol (50 g, 177 mmol) and triethylamine (19.73 g, 195 mmol) dissolved in 50 g of diethylether was prepared. A second solution comprising acryloyl chloride (17.65 g, 195 mmol) dissolved in 50 g of diethylether was added dropwise to the first solution followed by stirring for four hours at room temperature. The resulting solution was then added to water, and the organic phase was extracted. The organic phase was distilled to yield 48.38 g of TBEA (72.5% yield). was prepared was added dropwise to the first solution the organic phase was extracted The organic phase was distilled to yield 48.38 g of TBEA (72.5% yield)

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A first solution comprising tribromoethanol (50 g, 177 mmol) and triethylamine (19.73 g, 195 mmol) dissolved in 70 g of diethylether was prepared. A second solution comprising methacryloyl chloride (20.39 g, 195 mmol) dissolved in 70 g of diethylether was added dropwise to the first solution followed by stirring for four hours at room temperature. The resulting solution was then added to water, and the organic phase was extracted. The organic phase was distilled to yield 32.85 g of TBEMA (52.9% yield). was prepared was added dropwise to the first solution the organic phase was extracted The organic phase was distilled to yield 32.85 g of TBEMA (52.9% yield)

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A first solution including tribromoethanol (50 g, 177 mmol) and triethylamine (19.73 g, 195 mmol) dissolved in 50 g of diethylether was prepared. A second solution comprising acryloyl chloride (17.65 g, 195 mmol) dissolved in 50 g of diethylether was added dropwise to the first solution followed by stirring for four hours at room temperature. The resulting solution was then added to water, and the organic phase was extracted. The organic phase was distilled to yield 48.38 g of TBEA (72.5% yield). was prepared was added dropwise to the first solution the organic phase was extracted The organic phase was distilled to yield 48.38 g of TBEA (72.5% yield)

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Tribromoethanol (43.8 parts) was converted to the corresponding chloroformate by reaction with 40 parts of phosgene in the presence of a stoichiometric amount of base. The purified intermediate was reacted with an excess of sodium azide to produce the β,β,β-tribromoethyl azidoformate.

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Tribromoethanol (43.8 parts) was converted to the corresponding chloroformate by reaction with 40 parts of phosgene in the presence of a stoichiometric amount of base. The purified intermediate was reacted with an excess of sodium azide to produce the β,β,β-tribromoethyl azidoformate.