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4-Fluoroaniline → N-(4-(1-(4-methoxybenzyl)-3-methyl-1H-pyrazolo[3,4-b]pyridin-4-yloxy)phenyl)-N-(4-fluorophenyl)cyclopropane-1,1-dicarboxamide

HRID 2241200
ノート
印刷プレビュー

反応式

HRID 2241200 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9]([C:11]2([C:14]([OH:16])=O)[CH2:13][CH2:12]2)=[O:10])=[CH:4][CH:3]=1.C1(C(O)=O)(C(O)=O)CC1.FC1C=CC([NH2:31])=CC=1.C(Cl)(=O)C(Cl)=O.[CH3:40][O:41][C:42]1[CH:66]=[CH:65][C:45]([CH2:46][N:47]2[C:51]3=[N:52][CH:53]=[CH:54][C:55]([O:56][C:57]4[CH:62]=[CH:61][C:60](N)=[CH:59][CH:58]=4)=[C:50]3[C:49]([CH3:64])=[N:48]2)=[CH:44][CH:43]=1>C1COCC1.O.C([O-])(O)=O.[Na+].CN(C=O)C>[F:1][C:2]1[CH:3]=[CH:4][C:5]([N:8]([C:60]2[CH:59]=[CH:58][C:57]([O:56][C:55]3[CH:54]=[CH:53][N:52]=[C:51]4[N:47]([CH2:46][C:45]5[CH:44]=[CH:43][C:42]([O:41][CH3:40])=[CH:66][CH:65]=5)[N:48]=[C:49]([CH3:64])[C:50]=34)=[CH:62][CH:61]=2)[C:9]([C:11]2([C:14]([NH2:31])=[O:16])[CH2:12][CH2:13]2)=[O:10])=[CH:6][CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

10

反応物 5

HCID 97314-FluoroanilineHCID 65578Oxalyl chlorideHCID 690171,1-Cyclopropanedicarboxylic acidHCID 210815301-[(4-Fluorophenyl)carbamoyl]cyclopropanecarboxylic AcidHCID 685150574-(1-(4-methoxybenzyl)-3-methyl-1H-pyrazolo[3,4-b]pyridin-4-yloxy)aniline

生成物 1

HCID 68513243
N-(4-(1-(4-methoxybenzyl)-3-methyl-1H-pyrazolo[3,4-b]pyridin-4-yloxy)phenyl)-N-(4-fluorophenyl)cyclopropane-1,1-dicarboxamide
収率 28%

試薬・触媒・溶媒 4

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒HCID 8028Tetrahydrofuran溶媒2 回HCID 516892Sodium Bicarbonate溶媒

実験手順

A 100 mL round-bottomed flask was charged with 1-((4-fluorophenyl)carbamoyl)cyclopropane carboxylic acid (0.3516 g, 0.9767 mmol; prepared from cyclopropane-1,1-dicarboxylic acid and 4-fluoroaniline in THF (25 mL) using the methods of WO 2005/030140 and Shih and Rankin, Synth. Comm., 1996, 26(4), 833-836). Next, catalytic DMF (10 microliters) was added. While stirring oxalyl dichloride (0.08387 mL, 0.9767 mmol) was added. The reaction mixture was stirred for 30 minutes and 4-(1-(4-methoxybenzyl)-3-methyl-1H-pyrazolo[3,4-b]pyridin-4-yloxy)benzenamine (0.160 g, 0.3907 mmol) in THF (2 mL) was added. The reaction mixture was stirred for 1 hour, the diluted with water (50 mL) and saturated NaHCO3 (50 mL). The reaction mixture was extracted with EtOAc, washed with brine, dried organic over sodium sulfate, filtered and concentrated. The reaction mixture was purified by preparative TLC (0.5 mm) eluting with EtOAc. The product (90 mg, 28%) was obtained as a white solid. LRMS (esi pos) m/e 566 (M+1).

後処理

  1. additionwas added
  2. stirringThe reaction mixture was stirred for 1 hour
  3. extractionThe reaction mixture was extracted with EtOAc
  4. washwashed with brine, dried organic over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customThe reaction mixture was purified by preparative TLC (0.5 mm)
  8. washeluting with EtOAc

出典と根拠

ORDレコード
ord-32e250da6a0f4e76a2ec48c4ba7df900
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…

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