Tetrahydrofuran → HCID 66823861, compound

Temperature

50 °C

A mixture of dimethyl 3-(4-amino-1,3-dihydro-1-oxo-2H-isoindol-2-yl)-glutarate (5 g) and tetrahydrofuran (14 ml) in 20% potassium carbonate solution (45 ml) was stirred for 5 hours by heating up to 50° C. The aqueous phase was separated and concentrated to dryness under reduced pressure. The concentrate was stirred with methanol (50 ml) for 30 min. After filter, the filtrate concentrated to dryness and was mixed with isopropanol (50 ml) for crystal growing for 2 hours at room temperature. The resulting mixture was filtered and dried under reduced pressure to give 3.7 g of target yield as a white solid. yield: 81%. Melting point test showed that the product began to melt at 90° C. and the final melting point was not apparently observed.

1. customThe aqueous phase was separated
2. concentrationconcentrated to dryness under reduced pressure
3. stirringThe concentrate was stirred with methanol (50 ml) for 30 min
4. filtrationAfter filter
5. concentrationthe filtrate concentrated to dryness
6. additionwas mixed with isopropanol (50 ml) for crystal
7. waitgrowing for 2 hours at room temperature
8. filtrationThe resulting mixture was filtered
9. customdried under reduced pressure
10. customto give 3.7 g of target
11. customyield as a white solid
12. customto melt at 90° C.

ORD record

ord-8f6bbccb64ec4293b04ff55c7b65c9bd

Source dataset

uspto-grants-2015_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09085530B2