Triethylamine → HCID 68543674、化合物

HRID 2242176ノート

反応式

HRID 2242176 の反応式
[C:1]([CH2:4][N:5]1[C:9]([C:10]2[CH:15]=[C:14]([CH3:16])[CH:13]=[CH:12][C:11]=2O)=[C:8]([C:18]([OH:20])=[O:19])[CH:7]=[N:6]1)([OH:3])=O.CCN=C=N[CH2:26][CH2:27][CH2:28][N:29]([CH3:31])C.[CH2:32]([N:34](CC)CC)C.CN(C(ON1N=N[C:49]2[CH:50]=[CH:51]C=N[C:48]1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F>CN(C=O)C.O>[CH:27]1([CH2:28][NH:29][CH2:31][CH2:32][NH:34][C:1](=[O:3])[CH2:4][N:5]2[C:9]3[C:10]4[CH:15]=[C:14]([CH3:16])[CH:13]=[CH:12][C:11]=4[O:20][C:18](=[O:19])[C:8]=3[CH:7]=[N:6]2)[CH2:26][CH2:51][CH2:50][CH2:49][CH2:48]1

参加物

7

反応物 4

HCID 8471Triethylamine2 回HCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 136338384HCID 136338384、化合物

生成物 1

HCID 68543674HCID 68543674、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

Compound h was dissolved in DMF (2 mL) and to the solution was added EDCI and Triethylamine to the reaction mixture. The resultant solution was stirred for 6 h at rt. To the reaction mixture was then added HATU and triethyl amine and the reaction mixture was stirred further for another hour. After completion of the reaction, the reaction solution was diluted with water and extracted with ethyl acetate. The organic solution was dried over Na2SO4 and concentrated to provide the product i. The crude product was purified by Preparative TLC using 10% TEA in ethyl acetate as mobile phase: LC MS (Method B): 397 (M+l); 1H NMR (400 MHz, CDCl3/TMS):δ 8.24 (s, 1H), 7.60 (s, 1H), 7.37 (s, 2H), 6.47 (bs, 1H), 5.28 (s, 2H), 3.21 (q, J=5.5 Hz, 2H), 2.46 (s, 3H), 2.33 (t, J=5.1 Hz, 2H), 2.06-1.98 (m, 1H), 2.00 (s, 3H), 1.69-1.66 (m, 2H), 1.58-1.49 (m, 2H), 1.10-0.89 (m, 6H).

後処理

  1. customAfter completion of the reaction
  2. extractionextracted with ethyl acetate
  3. dry with materialThe organic solution was dried over Na2SO4
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-d2556332a23a464ea9e91bbf4ee02463
出典データセット
uspto-grants-2010_03
特許番号
US07671069B2

反応ノート

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