Hydrochloric Acid → Levobunolol Hydrochloride

HRID 22087

반응식

HRID 22087 반응식
[CH3:1][C:2]([NH:5][CH2:6][C@H:7]([OH:21])[CH2:8][O:9][C:10]1[CH:11]=[CH:12][CH:13]=[C:14]2[C:19](=[O:20])[CH2:18][CH2:17][CH2:16][C:15]=12)([CH3:4])[CH3:3].[ClH:22]>C(O)C>[CH3:4][C:2]([NH:5][CH2:6][C@H:7]([OH:21])[CH2:8][O:9][C:10]1[CH:11]=[CH:12][CH:13]=[C:14]2[C:19](=[O:20])[CH2:18][CH2:17][CH2:16][C:15]=12)([CH3:1])[CH3:3].[ClH:22]

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 39468Levobunolol

생성물 1

HCID 5284409Levobunolol Hydrochloride수율 51%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To the above toluenic solution containing levobunolol as free base, 16 ml ethanol and the stoichiometric amount of hydrogen chloride were added. The stirred mixture was cooled below 10° C. and kept at this temperature for one hour. The precipitated solid was filtered, washed with toluene, recrystallized twice from 43 ml ethanol and dried to give 10.0 g (51% yield) of levobunolol hydrochloride having a rotary power at 25° C. below -19°.

후처리

  1. temperatureThe stirred mixture was cooled below 10° C.
  2. filtrationThe precipitated solid was filtered
  3. washwashed with toluene
  4. customrecrystallized twice from 43 ml ethanol
  5. customdried

출처 및 근거

ORD 기록
ord-6a3b1f99d2ba4f2d923b4e3351667225
출처 데이터셋
uspto-grants-1995_06
특허 번호
US05426227

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