p-Toluenesulfonic acid monohydrate → N4-(5-cyclopropyl-1H-pyrazol-3-yl)pyrimidine-2,4-diamine

HRID 475177ノート

反応式

HRID 475177 の反応式
[CH:1]1([C:4]2[NH:8][N:7]=[C:6]([NH:9][C:10]3[CH:15]=[CH:14][N:13]=[C:12]([NH:16]CC4C=CC5N(C6CCCCO6)C=NC=5C=4)[N:11]=3)[CH:5]=2)[CH2:3][CH2:2]1.CC1C=CC(S(O)(=O)=O)=CC=1.O>CO.O>[CH:1]1([C:4]2[NH:8][N:7]=[C:6]([NH:9][C:10]3[CH:15]=[CH:14][N:13]=[C:12]([NH2:16])[N:11]=3)[CH:5]=2)[CH2:3][CH2:2]1

参加物

5

反応物 2

HCID 521998p-Toluenesulfonic acid monohydrateHCID 71272519N4-(5-cyclopropyl-1H-pyrazol-3-yl)-N2-((1-(tetrahydro-2H-pyran-2-yl)-1H-benzo[d]imidazol-5-yl)methyl)pyrimidine-2,4-diamine

生成物 1

HCID 86689872N4-(5-cyclopropyl-1H-pyrazol-3-yl)pyrimidine-2,4-diamine

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

To a solution of 32 (406 mg, 0.94 mmol) in MeOH (5 mL) and water (1 mL) was added p-TsOH.H2O (178 mg, 0.94 mmol). The reaction mixture was heated at reflux for 18 h. The solvent was evaporated under reduced pressure and the residue was purified by preparative HPLC to afford 180 mg (55%) of N2-41H-benzo[d]imidazol-5-yl)-methyl)-N4-(5-cyclopropyl-1H-pyrazol-3-yl)pyrimidine-2,4-diamine (I-13) as white solid.

後処理

  1. temperatureThe reaction mixture was heated
  2. temperatureat reflux for 18 h
  3. customThe solvent was evaporated under reduced pressure
  4. customthe residue was purified by preparative HPLC

出典と根拠

ORDレコード
ord-9e0624724cf84d34ba34efeac43952fb
出典データセット
uspto-grants-2014_01
特許番号
US08637537B2

反応ノート

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