Trifluoroacetic acid → 1-[(1R)-2-methoxy-1-phenylethyl]-3-[3-(1-methyl-1H-pyrazol-4-yl)-1H-pyrazolo[4,3-c]pyridin-6-yl]urea

HRID 571425ノート

反応式

HRID 571425 の反応式
[CH3:1][O:2][CH2:3][C@@H:4]([NH:11][C:12]([NH:14][C:15]1[N:20]=[CH:19][C:18]2[C:21]([C:43]3[CH:44]=[N:45][N:46]([CH3:48])[CH:47]=3)=[N:22][N:23](C(C3C=CC=CC=3)(C3C=CC=CC=3)C3C=CC=CC=3)[C:17]=2[CH:16]=1)=[O:13])[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1.FC(F)(F)C(O)=O.C([SiH](CC)CC)C>ClCCl>[CH3:1][O:2][CH2:3][C@H:4]([NH:11][C:12]([NH:14][C:15]1[N:20]=[CH:19][C:18]2[C:21]([C:43]3[CH:44]=[N:45][N:46]([CH3:48])[CH:47]=3)=[N:22][NH:23][C:17]=2[CH:16]=1)=[O:13])[C:5]1[CH:6]=[CH:7][CH:8]=[CH:9][CH:10]=1

参加物

5

反応物 3

HCID 6422Trifluoroacetic acidHCID 12052TriethylsilaneHCID 89525815(S)-1-(2-methoxy-1-phenylethyl)-3-(3-(1-methyl-1H-pyrazol-4-yl)-1-trityl-1H-pyrazolo[4,3-c]pyridin-6-yl)urea

生成物 1

HCID 895360651-[(1R)-2-methoxy-1-phenylethyl]-3-[3-(1-methyl-1H-pyrazol-4-yl)-1H-pyrazolo[4,3-c]pyridin-6-yl]urea収率 28%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To the solution of (S)-1-(2-methoxy-1-phenylethyl)-3-(3-(1-methyl-1H-pyrazol-4-yl)-1-trityl-1H-pyrazolo[4,3-c]pyridin-6-yl)urea (63.4 mg, 0.100 mmol) and trifluoroacetic acid (0.383 ml, 5.00 mmol) in Dichloromethane (2.0 ml) was added triethylsilane (17.45 mg, 0.150 mmol). The resulting mixture was allowed to stir at rt for 18 h. LC-MS showed the completion of the reaction. After concentration the residue was purified by reverse phase HPLC to provide desired product (17.3 mg, 0.028 mmol, 27.9% yield). MS ESI Calc'd for C20H21N7O2 [M+H]+ 392, found 392

後処理

  1. customthe completion of the reaction
  2. concentrationAfter concentration the residue
  3. customwas purified by reverse phase HPLC

出典と根拠

ORDレコード
ord-5c88136a63cc482abb213a880a94bdf5
出典データセット
uspto-grants-2015_05
特許番号
US09023865B2

反応ノート

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