Trifluoroacetic acid → HCID 11177225、化合物

HRID 1172572

反応式

HRID 1172572 の反応式
C(O)(C(F)(F)F)=O.[CH:8]12[CH2:14][CH:11]([NH:12][CH2:13]1)[CH2:10][N:9]2[C:15]1[N:20]=[C:19]([NH2:21])[N:18]2[N:22]=[C:23]([C:25]3[O:26][CH:27]=[CH:28][CH:29]=3)[N:24]=[C:17]2[CH:16]=1.Cl[CH2:31][C:32]1[C:33]([CH3:38])=[N:34][O:35][C:36]=1[CH3:37].CCN(CC)CC>CC#N>[CH3:38][C:33]1[C:32]([CH2:31][N:12]2[CH2:13][CH:8]3[CH2:14][CH:11]2[CH2:10][N:9]3[C:15]2[N:20]=[C:19]([NH2:21])[N:18]3[N:22]=[C:23]([C:25]4[O:26][CH:27]=[CH:28][CH:29]=4)[N:24]=[C:17]3[CH:16]=2)=[C:36]([CH3:37])[O:35][N:34]=1

参加物

6

反応物 4

HCID 6422Trifluoroacetic acidHCID 8471TriethylamineHCID 88246Isoxazole, 4-(chloromethyl)-3,5-dimethyl-HCID 686862367-(2,5-Diaza-bicyclo[2.2.1]hept-2-yl)-2-furan-2-yl-[1,2,4]triazolo[1,5-c]pyrimidin-5-ylamine

生成物 1

HCID 11177225HCID 11177225、化合物

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

The TFA salt of 7-(2,5-diaza-bicyclo[2.2.1]hept-2-yl)-2-furan-2-yl-[1,2,4]triazolo[1,5-c]pyrimidin-5-ylamine (0.3 mmol; see Example 18 above) was dissolved in 3 mL of CH3CN along with 0.3 mmol of 4-chloromethyl-3,5-dimethyl-isoxazole (Aldrich-Sigma, St. Louis, Mo.) and 0.5 mmol of Et3N. The reaction mixture was stirred at room temperature for 18 hours. It was then concentrated and purified by preparative HPLC to afford the title compound. 1H NMR (400 Hz, DMSO-d6) δ 7.80 (d, J=1.0 Hz, 1H), 7.00 (d, J=3.6 Hz, 1H), 6.60 (dd, J=3.6, 1.0 Hz, 1H), 5.7 (s, 1H), 4.80 (brs, 2H), 2.4-3.6 (m, 14H). MS m/z: 407 [M+H]+.

後処理

  1. concentrationIt was then concentrated
  2. custompurified by preparative HPLC

出典と根拠

ORDレコード
ord-ff1540c77f164a4ebdad0305a39bbe0a
出典データセット
uspto-grants-2010_11
特許番号
US07834014B2

関連ノート

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