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Pyrrole-2-Carboxylic Acid → HCID 59451446、化合物

HRID 1874846
ノート
印刷プレビュー

反応式

HRID 1874846 の反応式
CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.[Cl:25][C:26]1[CH:27]=[C:28]([CH:31]=[C:32]([O:34][C:35]2[C:40]([Cl:41])=[CH:39][CH:38]=[C:37]([CH2:42][NH:43][CH3:44])[C:36]=2[F:45])[CH:33]=1)[C:29]#[N:30].[NH:46]1[CH:50]=[CH:49][CH:48]=[C:47]1[C:51]([OH:53])=O.C([O-])(O)=O.[Na+]>CN(C=O)C.C(OCC)(=O)C>[Cl:41][C:40]1[CH:39]=[CH:38][C:37]([CH2:42][N:43]([CH3:44])[C:51]([C:47]2[NH:46][CH:50]=[CH:49][CH:48]=2)=[O:53])=[C:36]([F:45])[C:35]=1[O:34][C:32]1[CH:31]=[C:28]([C:29]#[N:30])[CH:27]=[C:26]([Cl:25])[CH:33]=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 12473Pyrrole-2-Carboxylic AcidHCID 516892Sodium BicarbonateHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 59451460HCID 59451460、化合物

生成物 1

HCID 59451446HCID 59451446、化合物収率 33.5%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

HATU (0.16 g, 0.43 mmol) was added to a solution of 3-chloro-5-({6-chloro-2-fluoro-3-[(methylamino)methyl]phenyl}oxy)benzonitrile (0.10 g, 0.30 mmol) and 1H-pyrrole-2-carboxylic acid (0.05 g, 0.43 mmol) in DMF (3 mL) and the solution was stirred at RT overnight. After 16 h, ethyl acetate (100 ml) and saturated NaHCO3 solution (100 ml) were added. The organic layer was separated, washed with saturated NaHCO3 solution (2×100 ml), brine (150 mL), dried over MgSO4, filtered and concentrated. The crude material was purified by Reverse Phase HPLC to give the title compound (0.042 g, 33%) as a white solid. 1H NMR (400 MHz, CDCl3) δ ppm 9.77 (d, 1H), 7.34-7.40 (m, 1H), 7.21-7.33 (m, 3H), 7.17 (t, 1H), 7.01-7.05 (m, 1H), 6.99 (d, 1H), 6.28 (d, 1H), 4.85 (br. s., 2H), 3.33 (br. s., 3H).

後処理

  1. waitAfter 16 h
  2. customThe organic layer was separated
  3. washwashed with saturated NaHCO3 solution (2×100 ml), brine (150 mL)
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customThe crude material was purified by Reverse Phase HPLC

出典と根拠

ORDレコード
ord-c77eb06b6fc147d89631cd8056051fbc
出典データセット
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08304419B2

反応ノート

読み込み中…

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