6-chloro-2-[4-(2-chlorophenyl)-2-{[5-(trifluoromethyl)-2H-tetrazol-2-yl]methyl}pyrimidin-5-yl]-8-methyl-4H-3,1-benzoxazin-4-one → N-[4-chloro-2-methyl-6-(methylcarbamoyl)phenyl]-4-(2-chlorophenyl)-2-{[5-(trifluoromethyl)-2H-tetrazol-2-yl]methyl}pyrimidine-5-carboxamide

HRID 874195ノート

反応式

HRID 874195 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH3:36])[C:5]2[N:10]=[C:9]([C:11]3[C:12]([C:27]4[CH:32]=[CH:31][CH:30]=[CH:29][C:28]=4[Cl:33])=[N:13][C:14]([CH2:17][N:18]4[N:22]=[N:21][C:20]([C:23]([F:26])([F:25])[F:24])=[N:19]4)=[N:15][CH:16]=3)[O:8][C:7](=[O:34])[C:6]=2[CH:35]=1.[CH3:37][NH2:38].C1COCC1>C1COCC1>[Cl:1][C:2]1[CH:35]=[C:6]([C:7](=[O:34])[NH:38][CH3:37])[C:5]([NH:10][C:9]([C:11]2[C:12]([C:27]3[CH:32]=[CH:31][CH:30]=[CH:29][C:28]=3[Cl:33])=[N:13][C:14]([CH2:17][N:18]3[N:22]=[N:21][C:20]([C:23]([F:26])([F:24])[F:25])=[N:19]3)=[N:15][CH:16]=2)=[O:8])=[C:4]([CH3:36])[CH:3]=1

参加物

4

反応物 2

HCID 585643856-chloro-2-[4-(2-chlorophenyl)-2-{[5-(trifluoromethyl)-2H-tetrazol-2-yl]methyl}pyrimidin-5-yl]-8-methyl-4H-3,1-benzoxazin-4-oneHCID 66615946Methylamine tetrahydrofuran

生成物 1

HCID 58564390N-[4-chloro-2-methyl-6-(methylcarbamoyl)phenyl]-4-(2-chlorophenyl)-2-{[5-(trifluoromethyl)-2H-tetrazol-2-yl]methyl}pyrimidine-5-carboxamide

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
45 °C

実験手順

100 mg (0.18 mmol) of 6-chloro-2-[4-(2-chlorophenyl)-2-{[5-(trifluoromethyl)-2H-tetrazol-2-yl]methyl}pyrimidin-5-yl]-8-methyl-4H-3,1-benzoxazin-4-one were initially charged in 3 ml of THF, and 0.234 ml (0.46 mmol) of a 2 molar methylamine/THF solution was added at RT. The reaction mixture was then stirred at 45° C. for 15 min. After cooling, the mixture was concentrated and purified chromatographically on silice gel using cyclohexane/ethyl acetate. 48 mg (40% of theory; content 89%) of the desired product were isolated.

後処理

  1. temperatureAfter cooling
  2. concentrationthe mixture was concentrated
  3. custompurified chromatographically on silice gel

出典と根拠

ORDレコード
ord-d5814ab048ea4cc88c80e043a6e9fe8a
出典データセット
uspto-grants-2015_03
特許番号
US08980886B2

反応ノート

読み込み中…