Dichloromethane → Trifluoroacetic acid

HRID 1920567노트

반응식

HRID 1920567 반응식
F[P-](F)(F)(F)(F)F.C(OC([N:15]1[CH2:18][CH:17]([C:19]([NH:21][CH2:22][CH2:23][N+:24]23[CH2:31][CH2:30][CH:27]([CH2:28][CH2:29]2)[C@@H:26]([O:32][C:33](=[O:48])[C:34]([OH:47])([C:41]2[CH:46]=[CH:45][CH:44]=[CH:43][CH:42]=2)[C:35]2[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=2)[CH2:25]3)=[O:20])[CH2:16]1)=O)(C)(C)C.[C:49]([OH:55])([C:51]([F:54])([F:53])[F:52])=[O:50].C(Cl)Cl>C(O)(C(F)(F)F)=O.C(Cl)Cl>[F:52][C:51]([F:54])([F:53])[C:49]([OH:55])=[O:50].[F:52][C:51]([F:54])([F:53])[C:49]([O-:55])=[O:50].[NH:15]1[CH2:18][CH:17]([C:19]([NH:21][CH2:22][CH2:23][N+:24]23[CH2:31][CH2:30][CH:27]([CH2:28][CH2:29]2)[C@@H:26]([O:32][C:33](=[O:48])[C:34]([OH:47])([C:41]2[CH:42]=[CH:43][CH:44]=[CH:45][CH:46]=2)[C:35]2[CH:36]=[CH:37][CH:38]=[CH:39][CH:40]=2)[CH2:25]3)=[O:20])[CH2:16]1

참가 물질

6

반응물 3

HCID 6344DichloromethaneHCID 6422Trifluoroacetic acidHCID 86639173HCID 86639173, 화합물

생성물 2

HCID 6422Trifluoroacetic acidHCID 67495520HCID 67495520, 화합물

시약·촉매·용매 1

HCID 21863450Trifluoroacetic acid methylene chloride용매

실험 절차

(R)-1-(2-[(1-tert-butoxycarbonyl-azetidine-3-carbonyl)-amino]ethyl]-3-(2-hydroxy-2,2-diphenyl-acetoxy)1-azonia-bicyclo[2.2.2]octane hexafluorophosphate is dissolved in TFA:DCM (1:1) (2 ml) and stirred at room temperature for 1 hour. TFA:DCM (2 ml) is added to the reaction mixture to complete the reaction. The solvent is removed in vacuo and purification of the crude residue by mass directed preparative HPLC eluting with water:acetonitrile:trifluoroacetic acid yields the titled compound.

후처리

  1. customthe reaction
  2. customThe solvent is removed in vacuo and purification of the crude residue by mass
  3. washeluting with water

출처 및 근거

ORD 기록
ord-fa1bc6ae09124f3780cfef0c34443ee0
출처 데이터셋
uspto-grants-2012_05
특허 번호
US08168654B2

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