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Trifluoroacetic acid → HCID 59304309、化合物

HRID 2241440
ノート
印刷プレビュー

反応式

HRID 2241440 の反応式
COC1C=CC(C[N:8]2[C:12]3=[N:13][CH:14]=[CH:15][C:16]([N:17]([CH2:42][CH2:43][N:44]4[CH2:49][CH2:48][O:47][CH2:46][CH2:45]4)[C:18]4[CH:23]=[CH:22][C:21]([NH:24][C:25]([C:27]5[C:28](=[O:40])[N:29]([C:33]6[CH:38]=[CH:37][C:36]([F:39])=[CH:35][CH:34]=6)[N:30]=[CH:31][CH:32]=5)=[O:26])=[CH:20][C:19]=4[F:41])=[C:11]3[CH:10]=[N:9]2)=CC=1.C(O)(C(F)(F)F)=O>>[F:41][C:19]1[CH:20]=[C:21]([NH:24][C:25]([C:27]2[C:28](=[O:40])[N:29]([C:33]3[CH:34]=[CH:35][C:36]([F:39])=[CH:37][CH:38]=3)[N:30]=[CH:31][CH:32]=2)=[O:26])[CH:22]=[CH:23][C:18]=1[N:17]([CH2:42][CH2:43][N:44]1[CH2:45][CH2:46][O:47][CH2:48][CH2:49]1)[C:16]1[CH:15]=[CH:14][N:13]=[C:12]2[NH:8][N:9]=[CH:10][C:11]=12
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

3

反応物 2

HCID 6422Trifluoroacetic acidHCID 68516410N-(4-((1-(4-methoxybenzyl)-1H-pyrazolo[3,4-b]pyridin-4-yl)(2-morpholinoethyl)amino)-3-fluorophenyl)-2-(4-fluorophenyl)-3-oxo-2,3-dihydropyridazine-4-carboxamide

生成物 1

HCID 59304309HCID 59304309、化合物収率 112.9%

反応条件

温度
60 °C

実験手順

N-(4-((1-(4-methoxybenzyl)-1H-pyrazolo[3,4-b]pyridin-4-yl)(2-morpholinoethyl)amino)-3-fluorophenyl)-2-(4-fluorophenyl)-3-oxo-2,3-dihydropyridazine-4-carboxamide (0.015 g, 0.02165 mmol) was dissolved in TFA (0.1668 ml, 2.165 mmol) and stirred at 60° C. for 18 hours. Excess TFA was evaporated, and the crude product was then resuspended in toluene and reconcentrated to remove trace TFA. The crude solid was then partitioned between EtOAc and NaHCO3. The organic layer was separated and dried over sodium sulfate. After filtration to remove sodium sulfate and concentration, the residual crude solid was taken up in a small amount of DCM and treated with 2N HCl in ether. The suspension was evaporated to dryness to give 14 mg (95%) of product as a brown solid. LRMS (apci pos): 573.3 (M+H)+.

後処理

  1. customExcess TFA was evaporated
  2. customto remove trace TFA
  3. customThe crude solid was then partitioned between EtOAc and NaHCO3
  4. customThe organic layer was separated
  5. dry with materialdried over sodium sulfate
  6. filtrationAfter filtration
  7. customto remove
  8. concentrationsodium sulfate and concentration
  9. additiontreated with 2N HCl in ether
  10. customThe suspension was evaporated to dryness

出典と根拠

ORDレコード
ord-4b7835fed37542fca5d2b373844d0a6b
出典データセット
uspto-grants-2010_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07723330B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート