6-(1,3-dioxoisoindol-2-yl)hexanoyl chloride

反応条件: temp:0.00; pressure:0.00; stir:

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

実験手順: A solution of 6-phthalimidohexanoyl chloride (2 g.) in dry toluene was added to an ethereal solution of diazoethane at -78° C. and the mixture was allowed to warm to room temperature and stand for 15 hours. On standing a solid crystallized out of solution. The reaction mixture was filtered and the filtrate evaporated to dryness giving 1.43 g. of yellow-green oil. This oil was then dissolved in acetone and concentrated hydrochloric acid added until effervescence ceased. The resulting yellow-brown solution was then evaporated to dryness and azeotroped three times with toluene to give N-(7-chloro-6-oxooctyl)phthalimide (1.4 g.) which was used without further purification. crystallized out of solution The reaction mixture was filtered the filtrate evaporated to dryness giving 1.43 g The resulting yellow-brown solution was then evaporated to dryness azeotroped three times with toluene

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

実験手順: A solution of 6-phthalimidohexanoyl chloride (2 g.) in dry toluene was added to an ethereal solution of diazoethane at -78° C. and the mixture was allowed to warm to room temperature and stand for 15 hours. On standing a solid crystallized out of solution. The reaction mixture was filtered and the filtrate evaporated to dryness giving 1.43 g. of yellow-green oil. This oil was then dissolved in acetone and concentrated hydrochloric acid added until effervescence ceased. The resulting yellow-brown solution was then evaporated to dryness and azeotroped three times with toluene to give N-(7-chloro-6-oxooctyl)phthalimide (1.4 g.) which was used without further purification. crystallized out of solution The reaction mixture was filtered the filtrate evaporated to dryness giving 1.43 g The resulting yellow-brown solution was then evaporated to dryness azeotroped three times with toluene

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

実験手順: The same procedure is used as for Compound I, using 2,4,6-triiodo-3-amino-benzoic acid as iodo starting marterial and ε-phthalimidocaproic acid chloride.

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

実験手順: The same procedure is used as for Compound I, using 2,4,6-triiodo-3-amino-benzoic acid as iodo starting material and ε-phthalimidocaproic acid chloride.

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

実験手順: The same procedure is used as for Compound I, using 2,4,6-triiodo-3-amino-benzoic acid as iodo starting material and ε-phthalimidocaproic acid chloride.

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

実験手順: The same procedure is used as for Compound I, using 2,4,6-triiodo-3-amino-benzoic acid as iodo starting material and ε-phthalimidocaproic acid chloride.

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

実験手順: A solution of 6-phthalimidohexanoyl chloride (2 g.) in dry toluene was added to an ethereal solution of diazoethane at -78° C. and the mixture was allowed to warm to room temperature and stand for 15 hours. On standing a solid crystallized out of solution. The reaction mixture was filtered and the filtrate evaporated to dryness giving 1.43 g. of yellow-green oil. This oil was then dissolved in acetone and concentrated hydrochloric acid added until effervescence ceased. The resulting yellow-brown solution was then evaporated to dryness and azeotroped three times with toluene to give N-(7-chloro-6-oxooctyl)phthalimide (1.4 g.) which was used without further purification. crystallized out of solution The reaction mixture was filtered the filtrate evaporated to dryness giving 1.43 g The resulting yellow-brown solution was then evaporated to dryness azeotroped three times with toluene

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

実験手順: A solution of 6-phthalimidohexanoyl chloride (2 g.) in dry toluene was added to an ethereal solution of diazoethane at -78° C. and the mixture was allowed to warm to room temperature and stand for 15 hours. On standing a solid crystallized out of solution. The reaction mixture was filtered and the filtrate evaporated to dryness giving 1.43 g. of yellow-green oil. This oil was then dissolved in acetone and concentrated hydrochloric acid added until effervescence ceased. The resulting yellow-brown solution was then evaporated to dryness and azeotroped three times with toluene to give N-(7-chloro-6-oxooctyl)phthalimide (1.4 g.) which was used without further purification. crystallized out of solution The reaction mixture was filtered the filtrate evaporated to dryness giving 1.43 g The resulting yellow-brown solution was then evaporated to dryness azeotroped three times with toluene

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

実験手順: A solution of 6-phthalimidohexanoyl chloride (2 g.) in dry toluene was added to an ethereal solution of diazoethane at -78° C. and the mixture was allowed to warm to room temperature and stand for 15 hours. On standing a solid crystallized out of solution. The reaction mixture was filtered and the filtrate evaporated to dryness giving 1.43 g. of yellow-green oil. This oil was then dissolved in acetone and concentrated hydrochloric acid added until effervescence ceased. The resulting yellow-brown solution was then evaporated to dryness and azeotroped three times with toluene to give N-(7-chloro-6-oxooctyl)phthalimide (1.4 g.) which was used without further purification. crystallized out of solution The reaction mixture was filtered the filtrate evaporated to dryness giving 1.43 g The resulting yellow-brown solution was then evaporated to dryness azeotroped three times with toluene

反応条件: temp:0.00; pressure:0.00; stir:

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

実験手順: The same procedure is used as for Compound I, using 2,4,6-triiodo-3-amino-benzoic acid as iodo starting marterial and ε-phthalimidocaproic acid chloride.