Hydrochloric Acid → 4687-08-5

Temperature

80 °C

To the residue prepared in STEP C above was added water (10 g) and a 36-38% HCl solution (60 g). The resulting biphasic mixture was stirred at 80° C. for between about 4 and about 8 hours (till completion of the hydrolysis as determined by HPLC) The resulting mixture was then cooled to 60° C. and toluene (125 mL) added. The aqueous phase was discarded and the organic phase washed with water (50 mL). Toluene (about 80 g) was removed by distillation to dry the organic phase. The resulting solution was then cooled to 70° C. and petrol ether 60/90 (250 mL) was added. The resulting solution was further cooled to 37° C. and seeded. The resulting mixture was stirred for 30 minutes at 37° C., the resulting suspension then cooled to 0° C. over about 2.5 hours. The precipitated crystals were filtered off and washed with a mixture of toluene (5 mL 0 and petrol ether 60/90 (9 mL) to yield wet product. The wet product was dried in a vacuum at 30° C. to yield the title compound as an off-white solid.

1. customtill completion of the hydrolysis
2. temperaturewas then cooled to 60° C.
3. washthe organic phase washed with water (50 mL)
4. customToluene (about 80 g) was removed by distillation
5. customto dry the organic phase
6. temperatureThe resulting solution was then cooled to 70° C.
7. additionpetrol ether 60/90 (250 mL) was added
8. temperatureThe resulting solution was further cooled to 37° C.
9. stirringThe resulting mixture was stirred for 30 minutes at 37° C.
10. temperaturethe resulting suspension then cooled to 0° C. over about 2.5 hours
11. filtrationThe precipitated crystals were filtered off
12. washwashed with a mixture of toluene (5 mL 0 and petrol ether 60/90 (9 mL)
13. customto yield wet product
14. customThe wet product was dried in a vacuum at 30° C.

ORD record

ord-11667b9b5cf5496e85a92abe7dfdf376

Source dataset

uspto-grants-2013_09

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08541614B2