Hydrochloric Acid → N2,N4-bis(4-ethoxyphenyl)-2,4-pyrimidinediamine

HRID 71351

反応式

HRID 71351 の反応式
Cl[C:2]1[N:7]=[C:6](Cl)[CH:5]=[CH:4][N:3]=1.[CH2:9]([O:11][C:12]1[CH:18]=[CH:17][C:15]([NH2:16])=[CH:14][CH:13]=1)[CH3:10].Cl>CCO.O>[CH2:9]([O:11][C:12]1[CH:18]=[CH:17][C:15]([NH:16][C:2]2[N:7]=[C:6]([NH:16][C:15]3[CH:17]=[CH:18][C:12]([O:11][CH2:9][CH3:10])=[CH:13][CH:14]=3)[CH:5]=[CH:4][N:3]=2)=[CH:14][CH:13]=1)[CH3:10]

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 90764-EthoxyanilineHCID 775312,4-Dichloropyrimidine

生成物 1

HCID 22061075N2,N4-bis(4-ethoxyphenyl)-2,4-pyrimidinediamine

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

反応条件

温度
75 °C

実験手順

To a solution of 2,4-dichloropyrimidine (0.015 g, 0.1 mmol) in EtOH (1 mL) was added 4-ethoxyaniline (0.034 g, 0.025 mmol) and heated in a sealed tube at 70-80° C. for 24 h. Upon cooling the reaction was diluted with H2O (10 mL), acidified with 2N HCl, the solid obtained was filtered, washed with H2O and dried to give N2,N4-bis(4-ethoxyphenyl)-2,4-pyrimidinediamine (R926069). 1H NMR (CD3OD): δ 7.63 (d, 1H), 7.45 (d, 2H), J=9 Hz), 7.32 (d, 2H, J=9.3 Hz), 6.95 (d, 2H, J=6.9 Hz), 6.87 (d, 2H, J=8.7 Hz), 6.23 (d, 1H, J=7.2 Hz), 4.04 (m, 4H), 1.38 (m, 6H); LCMS: ret. time: 25.91 min.; purity: 99.5%; MS (m/e): 351 (MH+).

後処理

  1. temperatureUpon cooling the reaction
  2. customthe solid obtained
  3. filtrationwas filtered
  4. washwashed with H2O
  5. customdried

出典と根拠

ORDレコード
ord-f812dd0fec34470f921eacc2b5cb6f97
出典データセット
uspto-grants-2014_09
特許番号
US08822685B2

関連ノート

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