tert-butyl 3-{[5-chloro-4-(2,5-dichloro-3-cyanophenoxy)-1H-1,2,3-benzotriazol-1-yl]methyl}-1H-pyrazolo[3,4-b]pyridine-1-carboxylate → HCID 178509925、化合物

HRID 505552ノート

反応式

HRID 505552 の反応式
[Cl:1][C:2]1[CH:27]=[CH:26][C:5]2[N:6]([CH2:9][C:10]3[C:18]4[C:13](=[N:14][CH:15]=[CH:16][CH:17]=4)[N:12](C(OC(C)(C)C)=O)[N:11]=3)[N:7]=[N:8][C:4]=2[C:3]=1[O:28][C:29]1[CH:34]=[C:33]([Cl:35])[CH:32]=[C:31]([C:36]#[N:37])[C:30]=1[Cl:38]>C(O)(C(F)(F)F)=O>[Cl:38][C:30]1[C:29]([O:28][C:3]2[C:4]3[N:8]=[N:7][N:6]([CH2:9][C:10]4[C:18]5[C:13](=[N:14][CH:15]=[CH:16][CH:17]=5)[NH:12][N:11]=4)[C:5]=3[CH:26]=[CH:27][C:2]=2[Cl:1])=[CH:34][C:33]([Cl:35])=[CH:32][C:31]=1[C:36]#[N:37]

参加物

3

反応物 1

HCID 68428123tert-butyl 3-{[5-chloro-4-(2,5-dichloro-3-cyanophenoxy)-1H-1,2,3-benzotriazol-1-yl]methyl}-1H-pyrazolo[3,4-b]pyridine-1-carboxylate

生成物 1

HCID 178509925HCID 178509925、化合物

試薬・触媒・溶媒 1

HCID 6422Trifluoroacetic acid溶媒

実験手順

tert-Butyl 3-{[5-chloro-4-(2,5-dichloro-3-cyanophenoxy)-1H-1,2,3-benzotriazol-1-yl]methyl}-1H-pyrazolo[3,4-b]pyridine-1-carboxylate (569 mg, 0.997 mmol) was dissolved in TFA (5 mL). After 20 minutes, the reaction mixture was concentrated under reduced pressure, and the resulting residue was purified by reverse phase chromatography eluting with 30-95% MeCN/H2O+0.1% TFA. Product fractions concentrated under reduced pressure to yield the title compound. 1H NMR (DMSO-d6) δ 8.53 (dd, J=4.4 Hz, J=1.6 Hz, 1H), 8.14 (dd, J=8.0 Hz, J=1.5 Hz, 1H), 8.04 (d, J=0.6 Hz, 1H), 7.89 (d, J=8.9 Hz, 1H), 7.79 (d, J=8.9 Hz, 1H), 7.44 (d, J=0.6 Hz, 1H), 7.21 (dd, J=8.0 Hz, J=4.5 Hz, 1H), 6.38 (d, 2H). HRMS (M+1)=470.0076

後処理

  1. concentrationthe reaction mixture was concentrated under reduced pressure
  2. customthe resulting residue was purified by reverse phase chromatography
  3. washeluting with 30-95% MeCN/H2O+0.1% TFA
  4. concentrationProduct fractions concentrated under reduced pressure

出典と根拠

ORDレコード
ord-d7d95ea8aad9476aad0cdc83ca4efebe
出典データセット
uspto-grants-2010_08
特許番号
US07781454B2

反応ノート

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