Hydrogen Bromide → Bupropion Hydrobromide

HRID 229562

반응식

HRID 229562 반응식
[CH3:1][CH:2]([NH:12][C:13]([CH3:16])([CH3:15])[CH3:14])[C:3]([C:5]1[CH:6]=[CH:7][CH:8]=[C:9]([Cl:11])[CH:10]=1)=[O:4].[BrH:17]>C(O)(C)C>[CH3:1][CH:2]([NH:12][C:13]([CH3:14])([CH3:16])[CH3:15])[C:3]([C:5]1[CH:6]=[CH:7][CH:8]=[C:9]([Cl:11])[CH:10]=1)=[O:4].[BrH:17]

참가 물질

4

반응물 2

HCID 260Hydrogen BromideHCID 444Bupropion

생성물 1

HCID 11984562Bupropion Hydrobromide수율 74.8%

시약·촉매·용매 1

HCID 3776Isopropanol용매

반응 조건

온도
32.5 °C

실험 절차

A 250 ml flask equipped with overhead stirrer and gas inlet was charged with 34 g of bupropion base and 138 ml of isopropanol. The solution was maintained under stirring while 13 g of gaseous HBr was introduced through the gas inlet in a time of 20′ while the internal temperature of the mixture raises from 25 to 40° C. During the gas addition a heavy white precipitate formed. At the end of the gas addition the temperature of the mixture was raised to reflux (80° C.), to get complete solution of the suspended solid. The temperature was then lowered to 25° C. in 1 hour and further lowered to 0-5° C. in 1 additional hour. The precipitate obtained was filtered and washed with 20 ml of cold isopropanol. The discharged wet solid was dried under vacuum (30 mmHg) in a static drier at 50° C. for 16 hours. 34 g of bupropion hydrobromide form I were obtained.

후처리

  1. customA 250 ml flask equipped with overhead stirrer and gas inlet
  2. temperatureThe solution was maintained
  3. additionDuring the gas addition a heavy white precipitate
  4. customformed
  5. additionAt the end of the gas addition the temperature of the mixture
  6. temperaturewas raised
  7. temperatureto reflux (80° C.)
  8. customto get complete solution of the suspended solid
  9. customfurther lowered to 0-5° C. in 1 additional hour
  10. customThe precipitate obtained
  11. filtrationwas filtered
  12. washwashed with 20 ml of cold isopropanol
  13. customThe discharged wet solid was dried under vacuum (30 mmHg) in a static drier at 50° C. for 16 hours

출처 및 근거

ORD 기록
ord-e1e11355078b4eb996a3cf06abc8ad24
출처 데이터셋
uspto-grants-2009_07
특허 번호
US07563823B2

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