反応式
[OH:1][C:2]1[N:6]([CH3:7])[N:5]=[C:4]([C:8]([OH:10])=O)[CH:3]=1.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.CN(C=O)C.[CH2:40]([O:42][C:43](=[O:63])[C@H:44]([OH:62])[CH2:45][C@H:46]([NH2:61])[CH2:47][C:48]1[CH:53]=[CH:52][C:51]([C:54]2[CH:59]=[CH:58][CH:57]=[C:56]([Cl:60])[CH:55]=2)=[CH:50][CH:49]=1)[CH3:41].CCN(C(C)C)C(C)C>>[CH2:40]([O:42][C:43](=[O:63])[C@H:44]([OH:62])[CH2:45][C@H:46]([NH:61][C:8]([C:4]1[CH:3]=[C:2]([OH:1])[N:6]([CH3:7])[N:5]=1)=[O:10])[CH2:47][C:48]1[CH:53]=[CH:52][C:51]([C:54]2[CH:59]=[CH:58][CH:57]=[C:56]([Cl:60])[CH:55]=2)=[CH:50][CH:49]=1)[CH3:41]参加物
6
反応物 5
HCID 6228Dimethylformamide
HCID 81531Diisopropylethylamine
HCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)
HCID 86682253(2R,4R)-4-amino-5-(3'-chlorobiphenyl-4-yl)-2-hydroxypentanoic acid ethyl ester
HCID 178481916HCID 178481916、化合物生成物 1
実験手順
5-Hydroxy-1-methyl-1h-pyrazole-3-carboxylic acid (122 mg, 862 μmol) and HATU (361 mg, 949 μmol) were combined in DMF (1.0 mL, 13 mmol) and stirred for 10 minutes. (2R,4R)-4-amino-5-(3′-chlorobiphenyl-4-yl)-2-hydroxypentanoic acid ethyl ester (30.0 mg, 86 μmol) and DIPEA (165 μL, 949 μmol) were added, and the resulting mixture was stirred at room temperature overnight. The mixture was then concentrated under reduced pressure and the residue was dissolved in 50% AcOH-water (1.5 mL), filtered, purified by reverse phase preparative HPLC, and lyophilized to yield the title compound (11.1 mg). MS m/z [M+H]+ calc'd for C24H26ClN3O5, 472.16. found 472.2.
後処理
- stirringthe resulting mixture was stirred at room temperature overnight
- concentrationThe mixture was then concentrated under reduced pressure
- dissolutionthe residue was dissolved in 50% AcOH-water (1.5 mL)
- filtrationfiltered
- custompurified by reverse phase preparative HPLC
出典と根拠
- ORDレコード
- ord-a1e22c1b7ca94f548df0a5cbf19ac39c
- 出典データセット
- uspto-grants-2015_08
- 特許番号
- US09108934B2
関連ノート
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