Hydrochloric Acid → H6RY8HR9LM

HRID 431026ノート

反応式

HRID 431026 の反応式
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

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 20607354HCID 20607354、化合物

生成物 1

HCID 9843521H6RY8HR9LM収率 85.3%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-193ede19d4104e5787a05cbd2b3cbbb1
出典データセット
uspto-grants-2003_12
特許番号
US06656952B2

反応ノート

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