Benzyl Alcohol → HCID 67303962, 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 %) as impurities was dissolved in 9 ml of isopropanol, followed by adding 240 mg of sulfuric acid under ice cold conditions. 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 was heated to 40° C., 209 mg of isopropanol was added and the concentrate was dissolved completely. After the solution was gradually cooled to 22° C., 207 mg of hexane was added, and then a seed crystal was further added, and the deposited crystal was filtered under reduced pressure. The resultant wet crystal was dried under reduced pressure, thereby obtaining 75 mg of dry crystal of (R)-3-benzyloxypyrrolidine sulfate (yield of 7%, purity of 99.9%). 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. dissolutionthe concentrate was dissolved completely
5. temperatureAfter the solution was gradually cooled to 22° C.
6. additiona seed crystal was further added
7. filtrationthe deposited crystal was filtered under reduced pressure
8. customThe resultant wet crystal was dried under reduced pressure

ORD record

ord-957d96bd69e140bf8e23ad02b837a064

Source dataset

uspto-grants-2012_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08247578B2