1,4'-Bipiperidine → 4-Piperidinopiperidine-1-carbonyl chloride

In a solution of Triphosgene (16.48 gm) in methylene chloride (200 ml) was added a solution of 4-piperidinopiperidine (20 g) in methylene chloride (200 ml) at 20-25° C. within 1-2 hours. Part of the methylene chloride was distilled off and acetonitrile was added. Further, methylene chloride and acetonitrile was distilled off completely until the temperature rises to 70° C. At room temperature fresh methylene chloride was added to the reaction mixture to make homogenous slurry followed by potassium carbonate (30-35 gm) and reaction mixture was stirred for 1-2 hours. The reaction mixture was filtered and subsequently the filtrate was concentrated. Hexane was added slowly into the reaction mixture under stirring. Solid compound so obtained was filtered, washed with hexane and dried under reduced pressure at about 40° C.

1. distillationPart of the methylene chloride was distilled off
2. additionacetonitrile was added
3. distillationFurther, methylene chloride and acetonitrile was distilled off completely until the temperature
4. customrises to 70° C
5. additionAt room temperature fresh methylene chloride was added to the reaction mixture
6. customfollowed by potassium carbonate (30-35 gm) and reaction mixture
7. filtrationThe reaction mixture was filtered
8. concentrationsubsequently the filtrate was concentrated
9. additionHexane was added slowly into the reaction mixture
10. stirringunder stirring
11. customSolid compound so obtained
12. filtrationwas filtered
13. washwashed with hexane
14. customdried under reduced pressure at about 40° C.

ORDレコード

ord-35a56feac27247e082cb52677a99834e

出典データセット

uspto-grants-2013_10

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08546573B2