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p-Fluorobenzoic acid 2-isopropylhydrazide → HCID 86711453、化合物

HRID 1401103
ノート
印刷プレビュー

反応式

HRID 1401103 の反応式
[CH2:1]([N:6]1[C:14]2[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=2)[C:8](/[CH:15]=[CH:16]/[C:17]([OH:19])=O)=[CH:7]1)[CH2:2][CH:3]([CH3:5])[CH3:4].[F:20][C:21]1[CH:33]=[CH:32][C:24]([C:25]([NH:27][NH:28][CH:29]([CH3:31])[CH3:30])=[O:26])=[CH:23][CH:22]=1.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.C(N(CC)C(C)C)(C)C>CN(C=O)C.CCOC(C)=O>[F:20][C:21]1[CH:33]=[CH:32][C:24]([C:25]([NH:27][N:28]([C:17](=[O:19])/[CH:16]=[CH:15]/[C:8]2[C:9]3[C:14](=[CH:13][CH:12]=[CH:11][CH:10]=3)[N:6]([CH2:1][CH2:2][CH:3]([CH3:4])[CH3:5])[CH:7]=2)[CH:29]([CH3:30])[CH3:31])=[O:26])=[CH:23][CH:22]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 18030p-Fluorobenzoic acid 2-isopropylhydrazideHCID 81531DiisopropylethylamineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 86711443HCID 86711443、化合物

生成物 1

HCID 86711453HCID 86711453、化合物

試薬・触媒・溶媒 2

HCID 6228
Dimethylformamide
溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

To solution containing (E)-3-(1-isopentyl-1H-indol-3-yl)acrylic acid (170 mg, 0.66 mmol), 4-fluoro-N′-isopropylbenzohydrazide (194.3 mg, 0.99 mmol) and HATU (376.4 mg, 0.99 mmol) dissolved in DMF (3.0 ml), N,N-diisopropylethylamine (DIPEA)(0.17 ml, 0.99 mmol) was slowly drop-wise added and stirred at room temperature for 12 hr. The reaction mixture was diluted with EtOAc, washed with water and brine, dried with anhydrous MgSO4, filtered, and concentrated under reduced pressure. The residue was separated through silica gel chromatography (30% EtOAc) for refinement and dried so that ivory (E)-4-fluoro-N′-(3-(1-isopentyl-1H-indol-3-yl)acryloyl)-N′-isopropylbenzohydrazide was obtained (160.0 mg, 55.7%).

後処理

  1. washwashed with water and brine
  2. dry with materialdried with anhydrous MgSO4
  3. filtrationfiltered
  4. concentrationconcentrated under reduced pressure
  5. customThe residue was separated through silica gel chromatography (30% EtOAc) for refinement
  6. dry with materialdried so that ivory (E)-4-fluoro-N′-(3-(1-isopentyl-1H-indol-3-yl)acryloyl)-N′-isopropylbenzohydrazide
  7. customwas obtained (160.0 mg, 55.7%)

出典と根拠

ORDレコード
ord-6cc0841ff9d84d668d6b2b862c4f8d5a
出典データセット
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08906952B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート