Hydrochloric Acid → HCID 67768990、化合物

HRID 1898913ノート

反応式

HRID 1898913 の反応式
[ClH:1].[CH2:2]([N:4]([C:22]1[CH:27]=[CH:26][CH:25]=[C:24]([C:28]([F:31])([F:30])[F:29])[CH:23]=1)[C:5]([C:7]1[C:8]([NH2:21])=[N:9][C:10]([N:13]2[CH2:17][C:16]([CH3:19])([CH3:18])[NH:15][C:14]2=[O:20])=[N:11][CH:12]=1)=[O:6])[CH3:3]>CCOCC.CC(C)=O>[ClH:1].[CH2:2]([N:4]([C:22]1[CH:27]=[CH:26][CH:25]=[C:24]([C:28]([F:31])([F:29])[F:30])[CH:23]=1)[C:5]([C:7]1[C:8]([NH2:21])=[N:9][C:10]([N:13]2[CH2:17][C:16]([CH3:19])([CH3:18])[NH:15][C:14]2=[O:20])=[N:11][CH:12]=1)=[O:6])[CH3:3]

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 3086669Opanixil

生成物 1

HCID 67768990HCID 67768990、化合物収率 92.7%

試薬・触媒・溶媒 2

HCID 180Acetone溶媒HCID 3283Diethyl Ether溶媒

実験手順

1.52 ml of a 6.6 molar solution of HCl in ether were added dropwise to a solution of 3.80 g (9 mmol) of 4-amino-2-(4,4-dimethyl-2-oxo-1-imidazolidinyl)-pyrimidine-5-carboxylic acid N-ethyl-N-(3-trifluoromethylphenyl)amide prepared as in Example 1 in 20 ml of acetone at room temperature, and the resulting suspension was stirred while cooling in ice for 20 minutes. The crystals were then filtered off with suction, washed with acetone and ether and dried in vacuo (6-7 mbar) at 100° for 10 hours. 3.83 g (=92.7% yield) of 4-amino-2-(4,4-dimethyl-2-oxo-1-imidazolidinyl)pyrimidine-5-carboxylic acid N-ethyl-N-(3-trifluoromethylphenyl)amide hydrochloride were obtained, melting point 264°-265° (decomposition).

後処理

  1. temperaturewhile cooling in ice for 20 minutes
  2. filtrationThe crystals were then filtered off with suction
  3. washwashed with acetone and ether
  4. customdried in vacuo (6-7 mbar) at 100° for 10 hours

出典と根拠

ORDレコード
ord-2fbe8d7b3297448b9d2576725e81a436
出典データセット
uspto-grants-1996_11
特許番号
US05571816

反応ノート

読み込み中…