Diisopropylethylamine → HCID 73052913、化合物

HRID 2275495ノート

反応式

HRID 2275495 の反応式
[CH3:1][O:2][N:3]1[CH:7]=[C:6]([C:8]([OH:10])=O)[N:5]=[N:4]1.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.[NH2:35][C@H:36]([CH2:45][C:46]1[CH:51]=[CH:50][C:49]([C:52]2[CH:57]=[C:56]([Cl:58])[CH:55]=[CH:54][C:53]=2[F:59])=[CH:48][CH:47]=1)[CH2:37][C@:38]([CH2:43][OH:44])([CH3:42])[C:39]([OH:41])=[O:40].CCN(C(C)C)C(C)C>CN(C=O)C>[Cl:58][C:56]1[CH:55]=[CH:54][C:53]([F:59])=[C:52]([C:49]2[CH:48]=[CH:47][C:46]([CH2:45][C@@H:36]([NH:35][C:8]([C:6]3[N:5]=[N:4][N:3]([O:2][CH3:1])[CH:7]=3)=[O:10])[CH2:37][C@:38]([CH2:43][OH:44])([CH3:42])[C:39]([OH:41])=[O:40])=[CH:51][CH:50]=2)[CH:57]=1

参加物

6

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 89964351HCID 89964351、化合物HCID 89964407HCID 89964407、化合物

生成物 1

HCID 73052913HCID 73052913、化合物収率 8.3%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

1-Methoxy-1H-[1,2,3]triazole-4-carboxylic acid (4.3 mg, 30 μmol) and HATU (11.4 mg, 30 μmol) were combined in DMF (1 mL) and stirred at room temperature for 15 minutes. (2S,4R)-4-amino-5-(5′-chloro-2′-fluorobiphenyl-4-yl)-2-hydroxymethyl-2-methylpentanoic acid (10 mg, 27 μmol) and DIPEA (14 μL, 82 μmol) were added, and the resulting mixture was stirred for 15 minutes at room temperature. The solvent was removed in vacuo and the residue was purified by preparative HPLC to yield the title compound (1.1 mg). MS m/z [M+H]+ calc'd for C23H24ClFN4O5, 491.14. found 491.2.

後処理

  1. stirringthe resulting mixture was stirred for 15 minutes at room temperature
  2. customThe solvent was removed in vacuo
  3. customthe residue was purified by preparative HPLC

出典と根拠

ORDレコード
ord-f092cf953f254993ac74b0dc02342e92
出典データセット
uspto-grants-2015_09
特許番号
US09126956B2

反応ノート

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