Ammonia → HCID 11735690, compound

A column was charged with 180 ml of a strongly acidic ion exchange resin (AMBERLITE IR120B Na, manufactured by Japan Organo). The ion exchange resin was used after converting it from sodium ion type to hydrogen ion type through a hydrochloric acid treatment. Next, 36.00 g (214 mmol) of 5-aminolevulinic acid hydrochloride was dissolved in 1800 ml of ion exchange water and passed through said column, and then 1000 ml of ion exchange water was passed through the same. Next, 1 N aqueous ammonia was slowly passed through the same to collect 594 ml of yellow eluate. The thus collected eluate was added to 33 ml of 60% nitric acid (HNO3 442 mmol) and concentrated using an evaporator. To the concentrated liquid, 400 ml of methyl acetate was added, followed by vigorously stirring with a stirrer and then the mixture was allowed to stand at 4° C. for 16 hours. The thus precipitated solid was recovered by suction filtration and washed with 500 ml of methyl acetate. The thus obtained solid was dried under reduced pressure for 12 hours to obtain 31.09 g (160 mmol) of the substance of interest. Its physical property data are shown below.

1. additionA column was charged with 180 ml of a strongly acidic ion exchange resin (AMBERLITE IR120B Na, manufactured by Japan Organo)
2. customto collect 594 ml of yellow eluate
3. concentrationconcentrated
4. customan evaporator
5. additionTo the concentrated liquid, 400 ml of methyl acetate was added
6. filtrationThe thus precipitated solid was recovered by suction filtration
7. washwashed with 500 ml of methyl acetate
8. customThe thus obtained solid was dried under reduced pressure for 12 hours
9. customto obtain 31.09 g (160 mmol) of the substance of interest

ORD record

ord-3ed8104fb69946ad81376a3ffc82be91

Source dataset

uspto-grants-2012_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08173839B2