Diethyl Ether → Serinol ketoprofen Hydrochloride

HRID 1359993노트

반응식

HRID 1359993 반응식
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]

참가 물질

6

반응물 4

HCID 3283Diethyl EtherHCID 8058HexaneHCID 21866389Hydrogen chloride-ethyl acetateHCID 86623045Boc-serinol ketoprofen2회

생성물 1

HCID 86623046Serinol ketoprofen Hydrochloride

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-eaa01563653c436caeac4284f6056bf6
출처 데이터셋
uspto-grants-2011_02
특허 번호
US07879817B2

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