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Diisopropylethylamine → HCID 44540317、化合物

HRID 1616046
ノート
印刷プレビュー

反応式

HRID 1616046 の反応式
[Br:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]([OH:10])=O)=[N:6][CH:7]=1.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.CCN(C(C)C)C(C)C.[NH:44]1[C:52]2[C:47](=[C:48]([C:53]3[CH:54]=[C:55]([NH2:62])[C:56]4[CH:57]=[N:58][NH:59][C:60]=4[CH:61]=3)[CH:49]=[CH:50][CH:51]=2)[CH:46]=[CH:45]1>CN(C=O)C>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]([NH:62][C:55]2[CH:54]=[C:53]([C:48]3[CH:49]=[CH:50][CH:51]=[C:52]4[C:47]=3[CH:46]=[CH:45][NH:44]4)[CH:61]=[C:60]3[C:56]=2[CH:57]=[N:58][NH:59]3)=[O:10])=[N:6][CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 81531DiisopropylethylamineHCID 6085445-Bromopyridine-2-carboxylic acidHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 582680196-(1H-indol-4-yl)-1H-indazol-4-amine

生成物 1

HCID 44540317HCID 44540317、化合物収率 41.3%

試薬・触媒・溶媒

1
HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 5-bromo-2-pyridinecarboxylic acid (980 mg, 4.83 mmol, available from Alfa Aesar) in DMF (15 ml) was added HATU (1840 mg, 4.83 mmol) and DIPEA (2.53 ml, 14.50 mmol). The mixture was stirred at room temperature for 30 mins then 6-(1H-indol-4-yl)-1H-indazol-4-amine (600 mg, 2.41 mmol) was added and the mixture stirred at room temperature overnight. The reaction mixture was concentrated in vacuo to approx. 5 ml volume and was applied to 2×50 g aminopropyl cartridges that had been pre-conditioned with MeOH. The reaction mixture remained on the cartridges for 2 h before being eluted with MeOH. The eluent was concentrated in vacuo and a precipitate formed, which was collected by filtration to give the title compound (430 mg) as a yellow solid.

後処理

  1. stirringthe mixture stirred at room temperature overnight
  2. concentrationThe reaction mixture was concentrated in vacuo to approx. 5 ml volume
  3. waitThe reaction mixture remained on the cartridges for 2 h
  4. washbefore being eluted with MeOH
  5. concentrationThe eluent was concentrated in vacuo
  6. customa precipitate formed
  7. filtrationwhich was collected by filtration

出典と根拠

ORDレコード
ord-a200f78a3806479c87cfb28b600280f6
出典データセット
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08765743B2

反応ノート

読み込み中…

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