Sodium Methoxide → 2-(2,4-Difluorophenyl)-4-(3-trifluoromethylphenyl)-5-meth anesulfonylpyrimidine

HRID 1653883ノート

反応式

HRID 1653883 の反応式
[F:1][C:2]([F:21])([F:20])[C:3]1[CH:4]=[C:5]([CH:17]=[CH:18][CH:19]=1)[C:6]([C:8]([S:13]([CH3:16])(=[O:15])=[O:14])=[CH:9]N(C)C)=O.Cl.[F:23][C:24]1[CH:32]=[C:31]([F:33])[CH:30]=[CH:29][C:25]=1[C:26]([NH2:28])=[NH:27].C[O-].[Na+]>CO>[F:23][C:24]1[CH:32]=[C:31]([F:33])[CH:30]=[CH:29][C:25]=1[C:26]1[N:28]=[C:6]([C:5]2[CH:17]=[CH:18][CH:19]=[C:3]([C:2]([F:1])([F:20])[F:21])[CH:4]=2)[C:8]([S:13]([CH3:16])(=[O:14])=[O:15])=[CH:9][N:27]=1

参加物

5

反応物 3

HCID 10942334Sodium MethoxideHCID 200809312,4-Difluoro-benzamidine hydrochlorideHCID 541640061-(3-trifluoromethylbenzoyl)-1-methanesulfonyl-2-(N,N-dimethylamino)ethene

生成物 1

HCID 150368532-(2,4-Difluorophenyl)-4-(3-trifluoromethylphenyl)-5-meth anesulfonylpyrimidine収率 77.5%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

6 g of 1-(3-trifluoromethylbenzoyl)-1-methanesulfonyl-2-(N,N-dimethylamino)ethene and 4.6 g of 2,4-difluorobenzamidine hydrochloride were dissolved in 30 ml of methanol at room temperature and 1.2 g of sodium methoxide was added thereto. The resulting mixture was heated under reflux for an hour. The solvent was distilled away under reduced pressure. The residue was washed with water and then dried to obtain 6 g of 2-(2,4-difluorophenyl)-4-(3-trifluoromethylphenyl)-5-meth anesulfonylpyrimidine (Compound 147).

後処理

  1. temperatureThe resulting mixture was heated
  2. temperatureunder reflux for an hour
  3. distillationThe solvent was distilled away under reduced pressure
  4. washThe residue was washed with water
  5. customdried

出典と根拠

ORDレコード
ord-5af1a966d7ca4c1585f20d8d497f9b61
出典データセット
uspto-grants-1995_04
特許番号
US05403948

反応ノート

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