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Trifluoroacetic acid → 3-(3-Aminophenoxy)-5-[(2-fluoro-4-iodophenyl)amino]isonicotinamide

HRID 2167223
ノート
印刷プレビュー

反応式

HRID 2167223 の反応式
[C:1]([C:4]1[C:9]([NH:10][C:11]2[CH:16]=[CH:15][C:14]([I:17])=[CH:13][C:12]=2[F:18])=[CH:8][N:7]=[CH:6][C:5]=1[O:19][C:20]1[CH:21]=[C:22]([NH:26]C(=O)OC(C)(C)C)[CH:23]=[CH:24][CH:25]=1)(=[O:3])[NH2:2].C(O)(C(F)(F)F)=O.C([O-])(O)=O.[Na+]>ClCCl>[NH2:26][C:22]1[CH:21]=[C:20]([CH:25]=[CH:24][CH:23]=1)[O:19][C:5]1[CH:6]=[N:7][CH:8]=[C:9]([NH:10][C:11]2[CH:16]=[CH:15][C:14]([I:17])=[CH:13][C:12]=2[F:18])[C:4]=1[C:1]([NH2:2])=[O:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6422Trifluoroacetic acidHCID 516892Sodium BicarbonateHCID 56970468Tert-butyl [3-({4-carbamoyl-5-[(2-fluoro-4-iodophenyl)amino]pyridin-3-yl}oxy)phenyl]carbamate

生成物 1

HCID 569704693-(3-Aminophenoxy)-5-[(2-fluoro-4-iodophenyl)amino]isonicotinamide収率 100%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

840 mg of tert-butyl [3-({4-carbamoyl-5-[(2-fluoro-4-iodophenyl)amino]pyridin-3-yl}oxy)phenyl]carbamate (1.488 mmol, 1 eq.) were dissolved in 8 mL dichloromethane under a nitrogen atmosphere. Then 1.6 ml of TFA were added and the brownish solution was stirred at room temperature for 18 hours. Then 4 ml of saturated aqueouse NaHCO3 solution was added and the mixture was stirred for 4 hours while a suspension was forming, that was filtered off. Drying of the precipitate in vacuo yielded 615 mg of the analytically pure target compound (1.488 mmol, 87% yield) as a yellowish solid.

後処理

  1. stirringthe mixture was stirred for 4 hours while a suspension
  2. customwas forming
  3. filtrationthat was filtered off
  4. customDrying of the precipitate in vacuo

出典と根拠

ORDレコード
ord-1eeaa369d3a440b5b570021e628bf8c1
出典データセット
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09045429B2

反応ノート

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