(6-Methylpyridin-2-yl)methanamine → N4-cyclohexyl-5,6-dimethyl-N2-[(6-methylpyridin-2-yl)methyl]pyrimidine-2,4-diamine

HRID 63110

反応式

HRID 63110 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.[CH3:25]C1N=C(CN)C=CC=1>>[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]=[C:21]([CH3:25])[N:20]=3)[N:10]=2)[CH2:3][CH2:4][CH2:5][CH2:6][CH2:7]1

参加物

3

反応物 2

HCID 246721(6-Methylpyridin-2-yl)methanamineHCID 131737202N4-cyclohexyl-5,6-dimethyl-N2-(pyridin-2-ylmethyl)pyrimidine-2,4-diamine hydrochloride

生成物 1

HCID 71738339N4-cyclohexyl-5,6-dimethyl-N2-[(6-methylpyridin-2-yl)methyl]pyrimidine-2,4-diamine

実験手順

The titled compound was synthesized according to the general procedure described for preparation of N4-cyclohexyl-5,6-dimethyl-N2-(pyridin-2-ylmethyl)pyrimidine-2,4-diamine (Example 1) using [(6-methylpyridin-2-yl)methyl]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 light-grey solid. 1H NMR (300 MHz, DMSO-d6) δ ppm 1.13-1.18 (m, 5H), 1.56-1.59 (m, 5H), 1.87 (s, 3H), 2.21 (s, 3H), 2.49 (s, 3H), 3.63 (d, J=6.72 Hz, 1H), 4.62 (d, J=4.30 Hz, 2H), 7.21-7.23 (m, 2H), 7.56 (d, J=5.64 Hz, 1H), 7.76-7.80 (m, 1H), 8.24 (s, 1H), 12.39 (s, 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-8d5e735131c74a2b9a7f77d69b5ebc88
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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