Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1) → HCID 25252912、化合物

HRID 914170ノート

反応式

HRID 914170 の反応式
[CH:1]1([N:6]2[CH2:12][C:11]([CH2:14][CH3:15])([F:13])[C:10](=[O:16])[N:9]([CH3:17])[C:8]3[CH:18]=[N:19][C:20]([NH:22][C:23]4[CH:31]=[CH:30][C:26]([C:27]([OH:29])=O)=[CH:25][C:24]=4[O:32][CH3:33])=[N:21][C:7]2=3)[CH2:5][CH2:4][CH2:3][CH2:2]1.CN(C(ON1N=[N:49][C:44]2[CH:45]=C[CH:47]=[N:48][C:43]1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.Cl.CN1CC(N)C1>>[CH:1]1([N:6]2[CH2:12][C:11]([CH2:14][CH3:15])([F:13])[C:10](=[O:16])[N:9]([CH3:17])[C:8]3[CH:18]=[N:19][C:20]([NH:22][C:23]4[CH:31]=[CH:30][C:26]([C:27]([NH:49][CH:44]5[CH2:43][N:48]([CH3:47])[CH2:45]5)=[O:29])=[CH:25][C:24]=4[O:32][CH3:33])=[N:21][C:7]2=3)[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 58214898HCID 58214898、化合物HCID 670505831-Methylazetidin-3-amine xhydrochloride

生成物 1

HCID 25252912HCID 25252912、化合物

実験手順

The title compound was synthesized from 4-(9-cyclopentyl-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 0.89 (t, J=7.3 Hz, 3H) 1.6-1.87 (m, 7H) 1.89-1.99 (m, 3H) 2.29 (s, 3H) 3.04 (t, J=7.1 Hz, 2H) 3.27 (s, 3H) 3.59 (t, J=7.2 Hz, 2H) 3.64-3.87 (m, 2H) 3.95 (s, 3H) 4.29-4.53 (m, 1H) 4.79 (t, J=8.1 Hz, 1H) 7.42-7.59 (m, 2H) 7.82 (s, 1H) 8.17 (s, 1H) 8.34 (d, J=8.3 Hz, 1H) 8.61 (d, J=6.8 Hz, 1H). [M+H] calc'd for C27H36FN7O3, 526. found 526.

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-54960f7ef8cc4a318691b79d7c999329
出典データセット
uspto-grants-2011_09
特許番号
US08026234B2

反応ノート

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