1-{3-[4-(2-aminopyrimidin-4-yl)-1-(4-methoxybenzyl)-1H-pyrazol-3-yl]phenyl}-3-[4-(trifluoromethyl)phenyl]urea → HCID 178508383、化合物

HRID 1843665ノート

反応式

HRID 1843665 の反応式
[NH2:1][C:2]1[N:7]=[C:6]([C:8]2[C:9]([C:22]3[CH:23]=[C:24]([NH:28][C:29]([NH:31][C:32]4[CH:37]=[CH:36][C:35]([C:38]([F:41])([F:40])[F:39])=[CH:34][CH:33]=4)=[O:30])[CH:25]=[CH:26][CH:27]=3)=[N:10][N:11](CC3C=CC(OC)=CC=3)[CH:12]=2)[CH:5]=[CH:4][N:3]=1>FC(F)(F)C(O)=O>[NH2:1][C:2]1[N:7]=[C:6]([C:8]2[C:9]([C:22]3[CH:23]=[C:24]([NH:28][C:29]([NH:31][C:32]4[CH:37]=[CH:36][C:35]([C:38]([F:39])([F:40])[F:41])=[CH:34][CH:33]=4)=[O:30])[CH:25]=[CH:26][CH:27]=3)=[N:10][NH:11][CH:12]=2)[CH:5]=[CH:4][N:3]=1

参加物

3

反応物 1

HCID 671848701-{3-[4-(2-aminopyrimidin-4-yl)-1-(4-methoxybenzyl)-1H-pyrazol-3-yl]phenyl}-3-[4-(trifluoromethyl)phenyl]urea

生成物 1

HCID 178508383HCID 178508383、化合物収率 73.2%

試薬・触媒・溶媒 1

HCID 6422Trifluoroacetic acid溶媒

反応条件

温度
70 °C

実験手順

800 mg (1.4 mmol) of 1-{3-[4-(2-aminopyrimidin-4-yl)-1-(4-methoxybenzyl)-1H-pyrazol-3-yl]phenyl}-3-[4-(trifluoromethyl)phenyl]urea were dissolved in 20 ml of trifluoroacetic acid and the mixture stirred at 70° C. for 4 hours. The solvent was then removed under reduced pressure and the residue taken up with dichloromethane and washed with aqueous sodium hydrogenocarbonate. The organic phase was dried over sodium sulphate and evaporated. The product was finally purified by flash-chromatography on a silica gel column (CH2Cl2-CH3OH; from 99/1 to 95/5), giving 450 mg (73%) of the title compound.

後処理

  1. customThe solvent was then removed under reduced pressure
  2. washwashed with aqueous sodium hydrogenocarbonate
  3. dry with materialThe organic phase was dried over sodium sulphate
  4. customevaporated
  5. customThe product was finally purified by flash-chromatography on a silica gel column (CH2Cl2-CH3OH; from 99/1 to 95/5)

出典と根拠

ORDレコード
ord-d53b1c644b6f40dc987ec76f753ec6c7
出典データセット
uspto-grants-2015_02
特許番号
US08946250B2

反応ノート

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