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Trifluoroacetic acid → 5-(2-benzyl-2H-indazol-6-yl)-7-(4-piperazin-1-ylphenyl)pyrrolo[2,1-f][1,2,4]triazin-4-amine

HRID 1972932
ノート
印刷プレビュー

反応式

HRID 1972932 の反応式
[NH2:1][C:2]1[C:7]2=[C:8]([C:30]3[CH:31]=[CH:32][C:33]4[C:37]([CH:38]=3)=[N:36][N:35]([CH2:39][C:40]3[CH:45]=[CH:44][CH:43]=[CH:42][CH:41]=3)[CH:34]=4)[CH:9]=[C:10]([C:11]3[CH:16]=[CH:15][C:14]([N:17]4[CH2:22][CH2:21][N:20](C(OC(C)(C)C)=O)[CH2:19][CH2:18]4)=[CH:13][CH:12]=3)[N:6]2[N:5]=[CH:4][N:3]=1.FC(F)(F)C(O)=O>ClCCl>[CH2:39]([N:35]1[CH:34]=[C:33]2[C:37]([CH:38]=[C:30]([C:8]3[CH:9]=[C:10]([C:11]4[CH:16]=[CH:15][C:14]([N:17]5[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]5)=[CH:13][CH:12]=4)[N:6]4[C:7]=3[C:2]([NH2:1])=[N:3][CH:4]=[N:5]4)[CH:31]=[CH:32]2)=[N:36]1)[C:40]1[CH:45]=[CH:44][CH:43]=[CH:42][CH:41]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 58529864tert-butyl 4-{4-[4-amino-5-(2-benzyl-2H-indazol-6-yl)pyrrolo[2,1-f][1,2,4]triazin-7-yl]phenyl}piperazine-1-carboxylate

生成物 1

HCID 585294985-(2-benzyl-2H-indazol-6-yl)-7-(4-piperazin-1-ylphenyl)pyrrolo[2,1-f][1,2,4]triazin-4-amine収率 96%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a suspension of tert-butyl 4-{4-[4-amino-5-(2-benzyl-2H-indazol-6-yl)pyrrolo[2,1-f][1,2,4]triazin-7-yl]phenyl}piperazine-1-carboxylate (610 mg, 1.02 mmol) in dichloromethane (6 mL) was added trifluoroacetic acid (2 mL). The reaction was stirred at rt for 17 h. The mixture was evaporated to dryness and saturated, aqueous NaHCO3 was added to the residue. The resulting solid was collected by filtration and was dried in vacuo to afford 489 mg (96%) of the desired product. 1H NMR (300 MHz, DMSO-d6) δ 8.54 (s, 1 H), 7.99-7.91 (m, 3 H), 7.81 (d, 1 H), 7.65 (s, 1 H), 7.41-7.25 (m, 5 H), 7.19 (d, 1 H), 7.06-6.96 (m, 3 H), 5.65 (s, 2 H), 3.14 (s, 4 H), 2.89 (s, 4 H); ES-MS m/z 501.4 [M+H]+, HPLC RT (min) 2.25.

後処理

  1. customThe mixture was evaporated to dryness
  2. additionsaturated, aqueous NaHCO3 was added to the residue
  3. filtrationThe resulting solid was collected by filtration
  4. customwas dried in vacuo

出典と根拠

ORDレコード
ord-5872432f3e374e3bb2f5d525b97d071a
出典データセット
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08431695B2

反応ノート

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