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Ammonia → HCID 44540892、化合物

HRID 244721
ノート
印刷プレビュー

反応式

HRID 244721 の反応式
[NH:1]1[CH:5]=[CH:4][N:3]=[C:2]1[C:6]([OH:8])=O.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.[NH:33]1[C:41]2[C:36](=[C:37]([C:42]3[CH:43]=[C:44]([NH2:57])[C:45]4[C:49]([CH:50]=3)=[N:48][N:47](C3CCCCO3)[CH:46]=4)[CH:38]=[CH:39][CH:40]=2)[CH:35]=[CH:34]1.CCN(C(C)C)C(C)C.N>CN(C=O)C.CO>[NH:33]1[C:41]2[C:36](=[C:37]([C:42]3[CH:50]=[C:49]4[C:45]([CH:46]=[N:47][NH:48]4)=[C:44]([NH:57][C:6]([C:2]4[NH:1][CH:5]=[CH:4][N:3]=4)=[O:8])[CH:43]=3)[CH:38]=[CH:39][CH:40]=2)[CH:35]=[CH:34]1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 222AmmoniaHCID 81531DiisopropylethylamineHCID 5743211H-Imidazole-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 582679956-(1H-Indol-4-yl)-2-(tetrahydro-2H-pyran-2-yl)-2H-indazol-4-amine

生成物 1

HCID 44540892
HCID 44540892、化合物

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 6228Dimethylformamide溶媒

実験手順

1H-Imidazole-2-carboxylic acid (17 mg) (available from Maybridge), HATU (63 mg) and 6-(1H-indol-4-yl)-2-(tetrahydro-2H-pyran-2-yl)-2H-indazol-4-amine (50 mg) were dissolved in anhydrous DMF (3 ml) and then treated with DIPEA (0.052 ml) and stirred at RT for 15 h. The mixture was treated with methanol (3 ml) and then macroporous-tosic acid resin (170 mg; 4.4 mmol/g) then stirred for 15 h. The mixture was then treated with 0.88 ammonia solution (0.600 ml), stirred for 10 min, then filtered and solvent blown off under a stream of nitrogen. The crude residue was purified by mass directed preparative HPLC (Method A) to give the title compound.

後処理

  1. stirringstirred for 10 min
  2. filtrationfiltered
  3. customThe crude residue was purified by mass

出典と根拠

ORDレコード
ord-1d9ce1e3f37046009054511e2b7b72ca
出典データセット
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08658635B2

反応ノート

読み込み中…

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