Diisopropylethylamine → Trifluoroacetic acid

HRID 1920551노트

반응식

HRID 1920551 반응식
[F:1][C:2]([F:7])([F:6])[C:3]([O-:5])=[O:4].[C:8]([CH2:11][N+:12]12[CH2:19][CH2:18][CH:15]([CH2:16][CH2:17]1)[C@@H:14]([O:20][C:21](=[O:36])[C:22]([OH:35])([C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1)[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1)[CH2:13]2)([OH:10])=O.CCN(C(C)C)C(C)C.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.Cl.[CH2:71]([C:73]1[CH:74]=[C:75]2[C:79](=[CH:80][C:81]=1[CH2:82][CH3:83])[CH2:78][CH:77]([NH2:84])[CH2:76]2)[CH3:72]>CN(C=O)C>[F:1][C:2]([F:7])([F:6])[C:3]([OH:5])=[O:4].[F:1][C:2]([F:7])([F:6])[C:3]([O-:5])=[O:4].[CH2:82]([C:81]1[CH:80]=[C:79]2[C:75](=[CH:74][C:73]=1[CH2:71][CH3:72])[CH2:76][CH:77]([NH:84][C:8]([CH2:11][N+:12]13[CH2:17][CH2:16][CH:15]([CH2:18][CH2:19]1)[CH:14]([O:20][C:21](=[O:36])[C:22]([OH:35])([C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1)[C:23]1[CH:24]=[CH:25][CH:26]=[CH:27][CH:28]=1)[CH2:13]3)=[O:10])[CH2:78]2)[CH3:83]

참가 물질

7

반응물 4

HCID 81531DiisopropylethylamineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 102361265,6-diethyl-2,3-dihydro-1H-inden-2-amine HydrochlorideHCID 86611356(R)-1-Carboxymethyl-3-(2-hydroxy-2,2-diphenyl-acetoxy)-1-azonia-bicyclo[2.2.2]-octane trifluoroacetate

생성물 2

HCID 6422Trifluoroacetic acidHCID 86639172(5,6-Diethyl-indan-2-ylcarbamoyl-methyl]-3-(2-hydroxy-2,2-diphenyl-acetoxy)-1-azonia-bicyclo[2.2.2]octane trifluoroacetate

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a stirred suspension of (R)-1-carboxymethyl-3-(2-hydroxy-2,2-diphenyl-acetoxy)-1-azonia-bicyclo[2.2.2]octane trifluoroacetate [Ex. 62] (0.052 g, 0.102 mmol) in dry DMF (5 ml) is added DIPEA (0.070 ml, 0.408 mmol), HATU (0.097 g, 0.255 mmol) and 5,6-Diethyl-indan-2-ylamine hydrochloride (0.058 g, 0.255 mmol). The mixture is left to stir at room temperature overnight. The solvent is removed in vacuo and purification by mass directed preparative HPLC eluting with acetonitrile:water:trifluoroacetic acid yields the titled compound.

후처리

  1. waitThe mixture is left
  2. customThe solvent is removed in vacuo and purification by mass
  3. washeluting with acetonitrile

출처 및 근거

ORD 기록
ord-c1c0347ae59249a297c783f5877baa0c
출처 데이터셋
uspto-grants-2012_05
특허 번호
US08168654B2

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