Diethyl Ether → Serinol ketoprofen Hydrochloride

HRID 1359993ノート

反応式

HRID 1359993 の反応式
C([NH:8][CH:9]([CH2:12][OH:13])[CH2:10][OH:11])(OC(C)(C)C)=O.[OH:14][C:15]([CH:17]([C:19]1[CH:32]=[CH:31][CH:30]=[C:21]([C:22]([C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)=[O:23])[CH:20]=1)[CH3:18])=[O:16].[ClH:33].C(OCC)(=O)C.C(OCC)C.CCCCCC>ClCCl>[NH2:8][CH:9]([CH2:12][OH:13])[CH2:10][OH:11].[ClH:33].[OH:16][C:15]([CH:17]([C:19]1[CH:32]=[CH:31][CH:30]=[C:21]([C:22]([C:24]2[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=2)=[O:23])[CH:20]=1)[CH3:18])=[O:14]

参加物

6

反応物 4

HCID 3283Diethyl EtherHCID 8058HexaneHCID 21866389Hydrogen chloride-ethyl acetateHCID 86623045Boc-serinol ketoprofen2 回

生成物 1

HCID 86623046Serinol ketoprofen Hydrochloride

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Boc-serinol-ketoprofen (0.428 mmol) was dissolved in dichloromethane (1 ml), and 4 N hydrochloric acid/ethyl acetate (4 ml) was added thereto under ice-cooling, followed by stirring for 2 hours while gradually returning to room temperature. After confirming disappearance of Boc-serinol-ketoprofen by TLC, diethyl ether and hexane were added thereto, and the resulting precipitate was centrifuged. The thus obtained precipitate was dried under reduced pressure to give the titled compound (243.6 mg, qu.). The structure was identified by 1H-NMR (CDCl3).

後処理

  1. temperatureunder ice-cooling
  2. customwhile gradually returning to room temperature
  3. additionwere added
  4. customThe thus obtained precipitate was dried under reduced pressure

出典と根拠

ORDレコード
ord-eaa01563653c436caeac4284f6056bf6
出典データセット
uspto-grants-2011_02
特許番号
US07879817B2

反応ノート

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