Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1) → 4-(9-Cyclohexyl-7-ethyl-7-fluoro-5-methyl-6-oxo-6,7,8,9-tetrahydro-5H-pyrimido[4,5-b][1,4]diazepin-2-ylamino)-3-methoxy-N-(1-methylazetidin-3-yl)benzamide

HRID 1880943ノート

反応式

HRID 1880943 の反応式
[CH:1]1([N:7]2[CH2:13][C:12]([CH2:15][CH3:16])([F:14])[C:11](=[O:17])[N:10]([CH3:18])[C:9]3[CH:19]=[N:20][C:21]([NH:23][C:24]4[CH:32]=[CH:31][C:27]([C:28](O)=[O:29])=[CH:26][C:25]=4[O:33][CH3:34])=[N:22][C:8]2=3)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.CN(C(ON1N=[N:50][C:45]2[CH:46]=C[CH:48]=[N:49][C:44]1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.Cl.CN1CC(N)C1>>[CH:1]1([N:7]2[CH2:13][C:12]([CH2:15][CH3:16])([F:14])[C:11](=[O:17])[N:10]([CH3:18])[C:9]3[CH:19]=[N:20][C:21]([NH:23][C:24]4[CH:32]=[CH:31][C:27]([C:28]([NH:50][CH:45]5[CH2:44][N:49]([CH3:48])[CH2:46]5)=[O:29])=[CH:26][C:25]=4[O:33][CH3:34])=[N:22][C:8]2=3)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1

参加物

4

反応物 3

HCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 670505831-Methylazetidin-3-amine xhydrochlorideHCID 67117835HCID 67117835、化合物

生成物 1

HCID 252530674-(9-Cyclohexyl-7-ethyl-7-fluoro-5-methyl-6-oxo-6,7,8,9-tetrahydro-5H-pyrimido[4,5-b][1,4]diazepin-2-ylamino)-3-methoxy-N-(1-methylazetidin-3-yl)benzamide

実験手順

The title compound was synthesized from 4-(9-cyclohexyl-7-ethyl-7-fluoro-5-methyl-6-oxo-6,7,8,9-tetrahydro-5H-pyrimido[5,4-b][1,4]diazepin-2-ylamino)-3-methoxybenzoic acid as described in the General procedure for amide bond synthesis using HATU and 1-methylazetidin-3-amine hydrochloride. The final compound was purified by reverse phase HPLC and basified to give the free base. 1H NMR (400 MHz, DMSO-d6) δ ppm 0.71-0.95 (m, 1 H) 0.89 (t, J=7.3 Hz, 3 H) 1.07-1.92 (m, 12 H) 2.29 (s, 3 H) 3.03 (t, J=7.1 Hz, 2 H) 3.26 (s, 3 H) 3.51-3.76 (m, 1 H) 3.58 (t, J=7.2 Hz, 2 H) 3.76-3.87 (m, 1 H) 3.95 (s, 3 H) 4.44 (m, 1 H) 7.49 (d, J=8.3 Hz, 1 H) 7.52 (s, 1 H) 7.78 (s, 1 H) 8.11 (s, 1 H) 8.33 (d, J=8.6 Hz, 1 H) 8.63 (d, J=6.8 Hz, 1 H). [M+H] calc'd for C28H38FN7O3, 540; found 540.

後処理

  1. customas described in the General procedure for amide bond synthesis
  2. customThe final compound was purified by reverse phase HPLC
  3. customto give the free base

出典と根拠

ORDレコード
ord-c0f199c42b1342b198e5cb0e4c678058
出典データセット
uspto-grants-2012_11
特許番号
US08318727B2

反応ノート

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