Triethylamine → HCID 68543674, 화합물

HRID 2242176노트

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HRID 2242176 반응식
[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

참가 물질

7

반응물 4

HCID 8471Triethylamine2회HCID 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, 화합물

생성물 1

HCID 68543674HCID 68543674, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-d2556332a23a464ea9e91bbf4ee02463
출처 데이터셋
uspto-grants-2010_03
특허 번호
US07671069B2

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