tetraethylazanium;fluoride;dihydrate

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

実験手順: A mixture of Dioxolane (B-5)(1.62 g), tetraethylammonium fluoride dihydrate (1.38 g) and acetic acid (0.5 ml) in tetrahydrofuran (10 ml) is stirred at room temperature for 2 hours. The reaction mixture is diluted with ethyl acetate (50 ml), washed with saturated saline, dried and concentrated. The residue purified by silica gel chromatography to give tilted Lactam (C-5)(895 mg) from the fractions eluted with benzene-ethyl acetate (1:5). washed with saturated saline dried concentrated The residue purified by silica gel chromatography to give eluted with benzene-ethyl acetate (1:5)

反応条件: temp:80.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: We have found that the presence of specific additives, not generally recognised as brighteners, in 2:1 chromium (III) chloride hexahydrate-choline chloride can significantly brighten the electrodeposit. For example when 10% of choline chloride is replaced by tetraethylammonium fluoride dihydrate or tetramethylammonium hydroxide pentahydrate thin semi-bright pale blue chromium deposits can be obtained. Approximately 6 ml of 2:1 chromium (III) chloride hexahydrate-[choline chloride (90%) tetraethylammonium fluoride dihydrate (10%)] was prepared by combining the reactants in a beaker and heating at 80° C. The green liquid was poured into an electrochemical cell (internal diameter of 23 mm) held in an oil bath at 60° C. Mild steel (50 mm by 10 mm and 1 mm thick), cleaned in the usual way, was fixed to the inside edge of the cell opposite a nickel counter electrode. The mild steel plate and counter-electrode were then connected to the negative and positive terminals respectively of a Thurlby Thander power pack. Using current densities between 8 and 16 mAcm−2 and deposition times between 10 and 30 minutes semi-bright chromium deposits were obtained. The procedure was repeated using approximately 6 ml of 2:1 chromium (III) chloride hexahydrate-[choline chloride (90%) tetramethylammonium hydroxide pentahydrate (10%)]. With a current density of 2 mAcm−2 thin pale blue semi-bright homogenous chromium deposits were obtained after 30 minutes. can be obtained The green liquid was poured into an electrochemical cell (internal diameter of 23 mm) held in an oil bath at 60° C

反応条件: temp:80.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: We have found that the presence of specific additives, not generally recognised as brighteners, in 2:1 chromium (III) chloride hexahydrate-choline chloride can significantly brighten the electrodeposit. For example when 10% of choline chloride is replaced by tetraethylammonium fluoride dihydrate or tetramethylammonium hydroxide pentahydrate thin semi-bright pale blue chromium deposits can be obtained. Approximately 6 ml of 2:1 chromium (III) chloride hexahydrate-[choline chloride (90%) tetraethylammonium fluoride dihydrate (10%)] was prepared by combining the reactants in a beaker and heating at 80° C. The green liquid was poured into an electrochemical cell (internal diameter of 23 mm) held in an oil bath at 60° C. Mild steel (50 mm by 10 mm and 1 mm thick), cleaned in the usual way, was fixed to the inside edge of the cell opposite a nickel counter electrode. The mild steel plate and counter-electrode were then connected to the negative and positive terminals respectively of a Thurlby Thander power pack. Using current densities between 8 and 16 mAcm−2 and deposition times between 10 and 30 minutes semi-bright chromium deposits were obtained. The procedure was repeated using approximately 6 ml of 2:1 chromium (III) chloride hexahydrate-[choline chloride (90%) tetramethylammonium hydroxide pentahydrate (10%)]. With a current density of 2 mAcm−2 thin pale blue semi-bright homogenous chromium deposits were obtained after 30 minutes. can be obtained The green liquid was poured into an electrochemical cell (internal diameter of 23 mm) held in an oil bath at 60° C

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

実験手順: A mixture of Dioxolane (B-5)(1.62 g), tetraethylammonium fluoride dihydrate (1.38 g) and acetic acid (0.5 ml) in tetrahydrofuran (10 ml) is stirred at room temperature for 2 hours. The reaction mixture is diluted with ethyl acetate (50 ml), washed with saturated saline, dried and concentrated. The residue purified by silica gel chromatography to give tilted Lactam (C-5)(895 mg) from the fractions eluted with benzene-ethyl acetate (1:5). washed with saturated saline dried concentrated The residue purified by silica gel chromatography to give eluted with benzene-ethyl acetate (1:5)

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

実験手順: A mixture of Dioxolane (B-5)(1.62 g), tetraethylammonium fluoride dihydrate (1.38 g) and acetic acid (0.5 ml) in tetrahydrofuran (10 ml) is stirred at room temperature for 2 hours. The reaction mixture is diluted with ethyl acetate (50 ml), washed with saturated saline, dried and concentrated. The residue purified by silica gel chromatography to give tilted Lactam (C-5)(895 mg) from the fractions eluted with benzene-ethyl acetate (1:5). washed with saturated saline dried concentrated The residue purified by silica gel chromatography to give eluted with benzene-ethyl acetate (1:5)

反応条件: temp:70.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 2-(trimethylsilyl)ethyl 4-((8-((5-cyano-4-((2-methoxyethyl)amino)pyridin-2-yl)carbamoyl)-2-(dimethoxymethyl)-5,6,7,8-tetrahydro-1,8-naphthyridin-3-yl)methyl)-3-oxopiperazine-1-carboxylate (intermediate 122, 4.20 g, 5.29 mmol) and tetraethylammonium fluoride dihydrate (2.53 g, 13.22 mmol) in AcCN (50 ml) was heated for 30 minutes at 70° C. The reaction mixture was partitioned between saturated aqueous NaHCO3 solution and DCM, the DCM phase washed with brine, dried over MgSO4 and evaporated. The residue was applied to a RediSep® silica column and purified by normal phase chromatography, eluting with EtOAc then a gradient from DCM to 10% MeOH in DCM. Product containing fractions were combined and evaporated to give the title compound as a yellow-white solid. (UPLC-MS 7) tR 0.68; ESI-MS 539.5 [M+H]+. The reaction mixture was partitioned between saturated aqueous NaHCO3 solution and DCM the DCM phase washed with brine dried over MgSO4 evaporated purified by normal phase chromatography eluting with EtOAc Product containing fractions evaporated

反応条件: temp:80.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: We have found that the presence of specific additives, not generally recognised as brighteners, in 2:1 chromium (III) chloride hexahydrate-choline chloride can significantly brighten the electrodeposit. For example when 10% of choline chloride is replaced by tetraethylammonium fluoride dihydrate or tetramethylammonium hydroxide pentahydrate thin semi-bright pale blue chromium deposits can be obtained. Approximately 6 ml of 2:1 chromium (III) chloride hexahydrate-[choline chloride (90%) tetraethylammonium fluoride dihydrate (10%)] was prepared by combining the reactants in a beaker and heating at 80° C. The green liquid was poured into an electrochemical cell (internal diameter of 23 mm) held in an oil bath at 60° C. Mild steel (50 mm by 10 mm and 1 mm thick), cleaned in the usual way, was fixed to the inside edge of the cell opposite a nickel counter electrode. The mild steel plate and counter-electrode were then connected to the negative and positive terminals respectively of a Thurlby Thander power pack. Using current densities between 8 and 16 mAcm−2 and deposition times between 10 and 30 minutes semi-bright chromium deposits were obtained. The procedure was repeated using approximately 6 ml of 2:1 chromium (III) chloride hexahydrate-[choline chloride (90%) tetramethylammonium hydroxide pentahydrate (10%)]. With a current density of 2 mAcm−2 thin pale blue semi-bright homogenous chromium deposits were obtained after 30 minutes. can be obtained The green liquid was poured into an electrochemical cell (internal diameter of 23 mm) held in an oil bath at 60° C

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

実験手順: A mixture of Dioxolane (B-5)(1.62 g), tetraethylammonium fluoride dihydrate (1.38 g) and acetic acid (0.5 ml) in tetrahydrofuran (10 ml) is stirred at room temperature for 2 hours. The reaction mixture is diluted with ethyl acetate (50 ml), washed with saturated saline, dried and concentrated. The residue purified by silica gel chromatography to give tilted Lactam (C-5)(895 mg) from the fractions eluted with benzene-ethyl acetate (1:5). washed with saturated saline dried concentrated The residue purified by silica gel chromatography to give eluted with benzene-ethyl acetate (1:5)