Hydrochloric Acid → H6RY8HR9LM

HRID 431026노트

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HRID 431026 반응식
Cl.C(OC([NH:9][C@H:10]1[C@@H:14]([CH2:15][F:16])[CH2:13][N:12]([C:17]2[C:26]([O:27][CH3:28])=[C:25]3[C:20]([C:21](=[O:35])[C:22]([C:32]([OH:34])=[O:33])=[CH:23][N:24]3[CH:29]3[CH2:31][CH2:30]3)=[CH:19][C:18]=2[F:36])[CH2:11]1)=O)(C)(C)C>O>[NH2:9][C@H:10]1[C@@H:14]([CH2:15][F:16])[CH2:13][N:12]([C:17]2[C:26]([O:27][CH3:28])=[C:25]3[C:20]([C:21](=[O:35])[C:22]([C:32]([OH:34])=[O:33])=[CH:23][N:24]3[CH:29]3[CH2:31][CH2:30]3)=[CH:19][C:18]=2[F:36])[CH2:11]1

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 20607354HCID 20607354, 화합물

생성물 1

HCID 9843521H6RY8HR9LM수율 85.3%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Concentrated hydrochloric acid (2 ml) was added to 7-[3-(S)-tert-butoxycarbonylamino-4-(S)-fluoromethyl-1-pyrrolidinyl]-1-cyclopropyl-6-fluoro-1,4-dihydro-8-methoxy-4-oxoquinoline -3-carboxylic acid (140 mg, 0.28 mmol) which was cooled in an ice bath, and the mixture was stirred for 30 minutes at the same temperature. The reaction solution was diluted with water (50 ml) and washed with chloroform (50 ml×3) and then, while cooling in an ice bath, the aqueous layer was alkalified with 50% sodium hydroxide aqueous solution. The aqueous layer was washed with dichloromethane (50 ml×3), adjusted to pH 7.4 with concentrated hydrochloric acid and 1N hydrochloric acid and then extracted with chloroform (100 ml×3). The organic layer was dried over sodium sulfate, the solvent was evaporated, and the thus obtained residue was purified by its recrystallization from a 28% aqueous ammonia-ethanol mixed solvent to give 94 mg (85%) of the title compound in the form of light yellow crystals.

후처리

  1. temperaturewas cooled in an ice bath
  2. washwashed with chloroform (50 ml×3)
  3. temperaturewhile cooling in an ice bath
  4. washThe aqueous layer was washed with dichloromethane (50 ml×3)
  5. extractionextracted with chloroform (100 ml×3)
  6. dry with materialThe organic layer was dried over sodium sulfate
  7. customthe solvent was evaporated
  8. customthe thus obtained residue was purified by its recrystallization from a 28% aqueous ammonia-ethanol mixed solvent

출처 및 근거

ORD 기록
ord-193ede19d4104e5787a05cbd2b3cbbb1
출처 데이터셋
uspto-grants-2003_12
특허 번호
US06656952B2

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