1-(Pyridin-2-yl)ethan-1-amine → N4-cyclohexyl-5,6-dimethyl-N2-[1-(pyridin-2-yl)ethyl]pyrimidine-2,4-diamine

HRID 63174

反応式

HRID 63174 の反応式
Cl.[CH:2]1([NH:8][C:9]2[C:14]([CH3:15])=[C:13]([CH3:16])[N:12]=[C:11]([NH:17][CH2:18][C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][N:20]=3)[N:10]=2)[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3]1.N1C=CC=C[C:26]=1C(N)C>>[CH:2]1([NH:8][C:9]2[C:14]([CH3:15])=[C:13]([CH3:16])[N:12]=[C:11]([NH:17][CH:18]([C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][N:20]=3)[CH3:26])[N:10]=2)[CH2:3][CH2:4][CH2:5][CH2:6][CH2:7]1

参加物

3

実験手順

The titled compound was synthesized according to the procedure described for preparation of N4-cyclohexyl-5,6-dimethyl-N2-(pyridin-2-ylmethyl)pyrimidine-2,4-diamine (Example 1) using (1-pyridin-2-ylethyl)amine instead of (pyridin-2-ylmethyl)amine. The product was purified by column chromatography eluting with mixture of chloroform/ethanol/20% water solution of ammonia (200:10:1), and then the final product was washed with diethyl ether to afford the titled compound as a white solid. 1H NMR (300 MHz, DMSO-d6) δ ppm 1.12-1.28 (m, 6H), 1.43-11.52 (m, 5H), 1.71-1.74 (m, 2H), 1.88 (s, 3H), 2.22 (s, 3H), 5.06-5.10 (m, 1H), 7.31 (t, J=8.06 Hz, 1H), 7.44 (d, J=8.06 Hz, 1H), 7.58 (d, J=8.06 Hz, 1H), 7.84 (t, J=8.06 Hz, 2H), 8.22 (d, J=2.0 Hz, 1H), 8.58 (d, J=2.0 Hz, 1H), 12.21 (bs, 1H); MS (ESI) m/z 326.5 (M+1)+.

後処理

  1. customThe titled compound was synthesized
  2. customThe product was purified by column chromatography
  3. washeluting with mixture of chloroform/ethanol/20% water solution of ammonia (200:10:1)
  4. washthe final product was washed with diethyl ether

出典と根拠

ORDレコード
ord-6c056cef9e88422292dc21a16b70b1e0
出典データセット
uspto-grants-2016_09
特許番号
US09447051B2

関連ノート

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