Hydrochloric Acid → Betaxolol Hydrochloride

HRID 1586272

반응식

HRID 1586272 반응식
[CH3:1][CH:2]([NH:4][CH2:5][CH:6]([OH:22])[CH2:7][O:8][C:9]1[CH:10]=[CH:11][C:12]([CH2:15][CH2:16][O:17][CH2:18][CH:19]2[CH2:21][CH2:20]2)=[CH:13][CH:14]=1)[CH3:3].[ClH:23]>C1(C)C=CC=CC=1.C(O)(C)C>[CH3:3][CH:2]([NH:4][CH2:5][CH:6]([OH:22])[CH2:7][O:8][C:9]1[CH:10]=[CH:11][C:12]([CH2:15][CH2:16][O:17][CH2:18][CH:19]2[CH2:21][CH2:20]2)=[CH:13][CH:14]=1)[CH3:1].[ClH:23]

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 2369Betaxolol

생성물 1

HCID 107952Betaxolol Hydrochloride수율 99%

시약·촉매·용매 2

HCID 1140Toluene용매HCID 3776Isopropanol용매

실험 절차

The oil obtained in Example 1 (179 grams) was dissolved in 400 mL of isopropylamine. After the reaction solution was refluxed for 2 days, the isopropylamine was distilled off and the residue was dissolved in 200 mL of toluene. The toluene was removed by vacuum distillation to give 222 grams of 1-{4-[2-(Cyclopropylmethoxy)ethyl]phenoxy}-3-isopropylamino-propane-2-ol (Betaxolol free base) which was used for the preparation of the hydrochloride salt without additional purification. The Betaxolol free base was dissolved in 300 mL of toluene containg 20 mL of isopropanol. A stream of hydrogen chloride gas was passed through the above solution at 0° C. until the reaction mixture pH was less than 3.0. The solvent was removed by vacuum distillation, and the residue was crystallized from 400 mL of acetone to give 102 grams (99% pure) of Betaxolol hydrochloride.

후처리

  1. customThe solvent was removed by vacuum distillation
  2. customthe residue was crystallized from 400 mL of acetone

출처 및 근거

ORD 기록
ord-4bf49b3677574b9c970f95986f248891
출처 데이터셋
uspto-grants-1999_08
특허 번호
US05942633

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