Acetonitrile → HCID 10340730、化合物

HRID 585997

反応式

HRID 585997 の反応式
[Cl:1][C:2]1[N:3]=[CH:4][C:5]2[C:10]([CH:11]=1)=[C:9]([N:12]=[C:13]=[O:14])[CH:8]=[CH:7][CH:6]=2.[N:15]1([C:21]2[CH:28]=[CH:27][C:24]([CH2:25][NH2:26])=[CH:23][CH:22]=2)[CH2:20][CH2:19][O:18][CH2:17][CH2:16]1.C(N(CC)CC)C.CC#N>C(OCC)C>[Cl:1][C:2]1[N:3]=[CH:4][C:5]2[C:10]([CH:11]=1)=[C:9]([NH:12][C:13]([NH:26][CH2:25][C:24]1[CH:23]=[CH:22][C:21]([N:15]3[CH2:20][CH2:19][O:18][CH2:17][CH2:16]3)=[CH:28][CH:27]=1)=[O:14])[CH:8]=[CH:7][CH:6]=2

参加物

6

反応物 4

HCID 6342AcetonitrileHCID 8471TriethylamineHCID 27764584-MorpholinobenzylamineHCID 22337685HCID 22337685、化合物

生成物 1

HCID 10340730HCID 10340730、化合物

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

The product from Example 176A in diethyl ether (40 mL) was treated with the product from Example 172B (300 mg, 1.56 mmol) and triethylamine (3 mL) in 1:1 diethyl ether:CH3CN (10 mL). After stirring for 3 hours, the mixture was filtered, and the collected solid was washed with diethyl ether. The solid was purified by silica gel chromatography (95:5 CH2Cl2:MeOH) to provide the title compound. 1H NMR (300 MHz, DMSO-d6) δ 9.18 (s, 1H), 8.71 (s, 1H), 8.37 (d, 1H, J=6.7 Hz), 8.08 (s, 1H), 7.79 (d, 2H, J=8.2 Hz), 7.63 (t, 1H, J=8.0 Hz), 7.23 (d, 2H, J=8.7 Hz), 6.94 (d, 2H, J=8.4 Hz), 6.91 (t, 1H, 5.5 Hz), 4.26 (d, 2H, 5.7 Hz), 3.73 (m, 4H), 3.07 (m, 4H); MS (ESI+) m/z 397/399 (M+H, 35Cl/37Cl).

後処理

  1. filtrationthe mixture was filtered
  2. washthe collected solid was washed with diethyl ether
  3. customThe solid was purified by silica gel chromatography (95:5 CH2Cl2:MeOH)

出典と根拠

ORDレコード
ord-1db545bf6a3d4ed09a1499399ec085d5
出典データセット
uspto-grants-2005_08
特許番号
US06933311B2

関連ノート

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