Benzyl Alcohol → HCID 67305675, compound

Temperature

40 °C

1.0 g of a concentrate containing (R)-3-benzyloxypyrrolidine obtained in Example 15 (purity of 86.6%) containing (R)-3-hydroxypyrrolidine (content of 0.12 wt %) and benzyl alcohol (content of 1.9 wt %) were contained as impurities were dissolved in 9 ml of isopropanol, followed by adding 0.82 g of 48% hydrobromic acid under ice cold condition. After stirring for a while, the mixture was concentrated and dried under reduced pressure, thereby obtaining a concentrate. After the concentrate was dispersed in 4.0 g of ethyl acetate and heated to 40° C. for complete dissolution, the solution was gradually cooled to 22° C. The deposited crystal was filtered under reduced pressure, and the resultant wet crystal was dried under reduced pressure, thereby obtaining 0.74 g of dry crystal of (R)-3-benzyloxypyrrolidine hydrobromide (yield of 59%, purity of 100.0%). Each of (R)-3-hydroxypyrrolidine and benzyl alcohol in the crystal was 0.01 wt % or less.

1. concentrationthe mixture was concentrated
2. customdried under reduced pressure
3. customobtaining a concentrate
4. temperaturethe solution was gradually cooled to 22° C
5. filtrationThe deposited crystal was filtered under reduced pressure
6. customthe resultant wet crystal was dried under reduced pressure

ORD record

ord-1503585d8cd8432f8536aee937d8a1f2

Source dataset

uspto-grants-2012_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08247578B2