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2-Chloro-4-iodoaniline → 3-[(2-Chloro-4-iodophenyl)amino]isonicotinic acid

HRID 39518
ノート
印刷プレビュー

反応式

HRID 39518 の反応式
F[C:2]1[CH:10]=[N:9][CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].C[Si]([N-][Si](C)(C)C)(C)C.[Li+].[Cl:21][C:22]1[CH:28]=[C:27]([I:29])[CH:26]=[CH:25][C:23]=1[NH2:24]>O1CCCC1>[Cl:21][C:22]1[CH:28]=[C:27]([I:29])[CH:26]=[CH:25][C:23]=1[NH:24][C:2]1[CH:10]=[N:9][CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=[O:5]
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 2829302-Chloro-4-iodoanilineHCID 3453613-Fluoropyridine-4-carboxylic acidHCID 2733832Lithium hexamethyldisilazane2 回

生成物 1

HCID 576496513-[(2-Chloro-4-iodophenyl)amino]isonicotinic acid

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To suspension of 3-fluoroisonicotinic acid (2.00 g, 14.17 mmol, in tetrahydrofuran (50 ml) at −78° C. was added lithium bis(trimethylsilyl)amide (14.3 ml, 17.01 mmol). The dark colored suspension was stirred for 15 min. In another flask, to a solution of 2-chloro-4-iodoaniline (4.7 g, 18.43 mmol) in THF (50 ml) was added lithium bis(trimethylsilyl)amide (24.9 ml, 29.77 mmol) at −78° C. under N2. The resulting green colored solution was stirred for 15 min. To this green colored solution the lithiated acid solution was added. The cold bath was removed, allowed to warm to room temperature, and stirred overnight. The mixture was filtered, and the crude was diluted with EtOAc (400 ml). It was then washed with dilute HCl (25 ml), H2O (25 ml), and dried. During concentration of the solvent, 3-[(2-chloro-4-iodophenyl)amino]isonicotinic acid was separated out as an yellow solid. (1.3 g, 24%)

後処理

  1. stirringThe resulting green colored solution was stirred for 15 min
  2. additionTo this green colored solution the lithiated acid solution was added
  3. customThe cold bath was removed
  4. stirringstirred overnight
  5. filtrationThe mixture was filtered
  6. additionthe crude was diluted with EtOAc (400 ml)
  7. washIt was then washed with dilute HCl (25 ml), H2O (25 ml)
  8. customdried
  9. customDuring concentration of the solvent, 3-[(2-chloro-4-iodophenyl)amino]isonicotinic acid was separated out as an yellow solid

出典と根拠

ORDレコード
ord-67a1f29fed714bb4aa9e2cab3928e5b7
出典データセット
uspto-grants-2013_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08524911B2

反応ノート

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