Hydrochloric Acid → 1-Methyl-3-phenylpiperazine

Compound (I) of the previous example (0.5 g, 2.077 mmol) and tetrahydrofurane (5 mL) were placed in a 25 mL flask, and for approximately 10 minutes the BH3.THF complex 1 M (10.4 mL, 10.386 mmol) was added to the white suspension. The resulting colourless solution was heated to reflux temperature for 6.5 hours, it was cooled to 19°±1° C. and an aqueous solution of HCl 6 N (1.82 mL) was added slowly. The mixture was distilled at reduced pressure to remove the tetrahydrofurane. Ethyl acetate (5 mL) was added and was extracted with an aqueous solution of HCl 2 N (3×5 mL). The accumulated acidic phases were alkalinised with an aqueous solution of NaOH 50% (p/p) to pH 12-13 (1.1 mL), saturated with NaCl (6.25 g) and were extracted with ethyl acetate (3×5 mL). The accumulated organic phases were dried with anhydrous Na2SO4, they were filtered and evaporated at reduced pressure, giving a yellowish liquid residue which corresponded to the title product (0.3 g, 81.97%).

1. additionfor approximately 10 minutes the BH3.THF complex 1 M (10.4 mL, 10.386 mmol) was added to the white suspension
2. temperatureThe resulting colourless solution was heated
3. temperatureto reflux temperature for 6.5 hours
4. temperatureit was cooled to 19°±1° C.
5. distillationThe mixture was distilled at reduced pressure
6. customto remove the tetrahydrofurane
7. additionEthyl acetate (5 mL) was added
8. extractionwas extracted with an aqueous solution of HCl 2 N (3×5 mL)
9. extractionwere extracted with ethyl acetate (3×5 mL)
10. dry with materialThe accumulated organic phases were dried with anhydrous Na2SO4, they
11. filtrationwere filtered
12. customevaporated at reduced pressure
13. customgiving a yellowish liquid residue which

ORD 기록

ord-c97014b0988e47aab92876b5371ff29e

출처 데이터셋

uspto-grants-2007_09

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US07265223B2