Hydrochloric Acid → Amoxicillin Trihydrate

HRID 610452

반응식

HRID 610452 반응식
[CH3:1][C:2]1([CH3:25])[S:6][C@@H:5]2[C@H:7]([NH:10][C:11]([C@H:13]([NH2:21])[C:14]3[CH:15]=[CH:16][C:17]([OH:20])=[CH:18][CH:19]=3)=[O:12])[C:8](=[O:9])[N:4]2[C@H:3]1[C:22]([OH:24])=[O:23].Cl>>[CH3:1][C:2]1([CH3:25])[S:6][C@@H:5]2[C@H:7]([NH:10][C:11]([C@H:13]([NH2:21])[C:14]3[CH:15]=[CH:16][C:17]([OH:20])=[CH:18][CH:19]=3)=[O:12])[C:8](=[O:9])[N:4]2[C@H:3]1[C:22]([OH:24])=[O:23].[OH2:9].[OH2:9].[OH2:9]

참가 물질

3

반응물 2

HCID 313Hydrochloric AcidHCID 33613Amoxicillin

생성물 1

HCID 62883Amoxicillin Trihydrate수율 88.4%

실험 절차

The solution obtained in step a) is added dropwise to the mixture obtained in step b) at a temperature of -45/-30°. The mixture is stirred for 90 minutes at a temperature of -30/-15°. The resultant crude protected amoxicillin mixture is worked up by treatment with a mixture of ice-water and concentrated hydrochloric acid and stirring for 30 minutes while cooling with ice. The aqueous phase is separated off and the organic phase reextracted with water. The combined aqueous phases are treated with concentrated aqueous sodium hydroxide to a pH of 4.5/5.5. Crystalline amoxicillin trihydrate is isolated as described in Example 10 c). Yield 88.4%. Purity 99.3%.

후처리

  1. stirringstirring for 30 minutes
  2. temperaturewhile cooling with ice
  3. customThe aqueous phase is separated off
  4. additionThe combined aqueous phases are treated with concentrated aqueous sodium hydroxide to a pH of 4.5/5.5

출처 및 근거

ORD 기록
ord-eae9812d476c4887b2977b5e6de8d9a1
출처 데이터셋
uspto-grants-1999_12
특허 번호
US05998610

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