Diisopropylethylamine → Trifluoroacetic acid

HRID 1920552ノート

反応式

HRID 1920552 の反応式
[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]

参加物

7

反応物 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

生成物 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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

Alternatively, 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 (0.053 ml, 0.306 mmol), HATU (0.058 g, 0.153 mmol) and 5,6-Diethyl-indan-2-ylamine hydrochloride (0.035 g, 0.153 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.

後処理

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

出典と根拠

ORDレコード
ord-9c4b633503f84b779ab56bdf5158a4dd
出典データセット
uspto-grants-2012_05
特許番号
US08168654B2

反応ノート

読み込み中…