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Triethylamine → 3,4-difluoro-2-(2-fluoro-4-iodo-phenylamino)-N-(2-hydroxy-ethoxy)-5-(2-oxo-tetrahydro-pyrimidin-1-ylmethyl)-benzamide

HRID 20779
ノート
印刷プレビュー

反応式

HRID 20779 の反応式
[NH2:1][CH2:2][CH2:3][CH2:4][NH:5][CH2:6][C:7]1[C:8]([F:30])=[C:9]([F:29])[C:10]([NH:20][C:21]2[CH:26]=[CH:25][C:24]([I:27])=[CH:23][C:22]=2[F:28])=[C:11]([CH:19]=1)[C:12]([NH:14][O:15][CH2:16][CH2:17][OH:18])=[O:13].C1C(=O)N(OC(ON2C(=O)CCC2=O)=O)[C:33](=[O:34])C1.C(N(CC)CC)C>C1COCC1.CC#N>[F:29][C:9]1[C:10]([NH:20][C:21]2[CH:26]=[CH:25][C:24]([I:27])=[CH:23][C:22]=2[F:28])=[C:11]([CH:19]=[C:7]([CH2:6][N:5]2[CH2:4][CH2:3][CH2:2][NH:1][C:33]2=[O:34])[C:8]=1[F:30])[C:12]([NH:14][O:15][CH2:16][CH2:17][OH:18])=[O:13]
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 8471TriethylamineHCID 676246Di(succinimido) carbonateHCID 593479915-[(3-amino-propylamino)-methyl]-3,4-difluoro-2-(2-fluoro-4-iodo-phenylamino)-N-(2-hydroxy-ethoxy)-benzamide

生成物 1

HCID 115704243,4-difluoro-2-(2-fluoro-4-iodo-phenylamino)-N-(2-hydroxy-ethoxy)-5-(2-oxo-tetrahydro-pyrimidin-1-ylmethyl)-benzamide収率 61.2%

試薬・触媒・溶媒 1

HCID 22177404
Acetonitrile tetrahydrofuran
溶媒

実験手順

The amine synthesized in Step A (66.4 mg, 0.1233 mmol) was dissolved in THF:CH3CN (1:1 v/v, 3.0 ml). N,N-disuccinimidyl carbonate (47.4 mg, 1.5 eq., 0.1849 mmol) and triethylamine (103.1 μl, 6.0 eq., 0.7398 mmol) were added sequentially to this solution, and the mixture was stirred at room temperature for 20 hours. The solvent was removed under reduced pressure, and the residue was purified by LC/MS to give white crystals (42.6 mg).

後処理

  1. customThe solvent was removed under reduced pressure
  2. customthe residue was purified by LC/MS

出典と根拠

ORDレコード
ord-187687b8fb3d433684e8cd7fd4d0ba73
出典データセット
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07745663B2

反応ノート

読み込み中…

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