(3-Trifluoromethylphenyl)urea → HCID 59684832、化合物

HRID 421808ノート

反応式

HRID 421808 の反応式
[F:1][C:2]([F:14])([F:13])[C:3]1[CH:4]=[C:5]([NH:9][C:10]([NH2:12])=[O:11])[CH:6]=[CH:7][CH:8]=1.[C:15]([C:17]1[CH:24]=[CH:23][C:20]([CH:21]=O)=[CH:19][CH:18]=1)#[N:16].[Br:25][C:26]1[CH:31]=[CH:30][C:29]([C:32](=[O:37])[CH2:33][C:34](=O)[CH3:35])=[CH:28][CH:27]=1>O1CCCC1>[Br:25][C:26]1[CH:27]=[CH:28][C:29]([C:32]([C:33]2[CH:21]([C:20]3[CH:23]=[CH:24][C:17]([C:15]#[N:16])=[CH:18][CH:19]=3)[NH:12][C:10](=[O:11])[N:9]([C:5]3[CH:6]=[CH:7][CH:8]=[C:3]([C:2]([F:13])([F:14])[F:1])[CH:4]=3)[C:34]=2[CH3:35])=[O:37])=[CH:30][CH:31]=1

参加物

5

反応物 3

HCID 25712(3-Trifluoromethylphenyl)ureaHCID 660424-CyanobenzaldehydeHCID 4326531-(4-bromophenyl)butane-1,3-dione

生成物 1

HCID 59684832HCID 59684832、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

4.23 g (20.74 mmol) N-[3-(trifluoromethyl)phenyl]urea, 2.72 g (20.74 mmol) 4-cyanobenzaldehyde, 5.00 g (20.74 mmol) 1-(4-bromophenyl)butane-1,3-dione and 6.5 g polyphosphoric acid ethyl ester are suspended in 50 ml of tetrahydrofuran. The mixture is stirred at reflux for 20 hours. After cooling down to room temperature, the solvent is removed in vacuo and the residue is purified by column chromatography on silica with cyclohexane/ethyl acetate mixtures as eluent.

後処理

  1. temperatureat reflux for 20 hours
  2. customthe solvent is removed in vacuo
  3. customthe residue is purified by column chromatography on silica with cyclohexane/ethyl acetate

出典と根拠

ORDレコード
ord-b6ef96fb8dfa4df8b48d39d5d0ee7d67
出典データセット
uspto-grants-2012_01
特許番号
US08101615B2

反応ノート

読み込み中…