p-(Trifluoromethoxy)phenyl isocyanate → Ethyl 1-methyl-4-[({[4-(trifluoromethoxy)phenyl]amino}carbonyl)amino]-1H-imidazole-2-carboxylate

HRID 2074073ノート

反応式

HRID 2074073 の反応式
[F:1][C:2]([F:14])([F:13])[O:3][C:4]1[CH:9]=[CH:8][C:7]([N:10]=[C:11]=[O:12])=[CH:6][CH:5]=1.[NH2:15][C:16]1[N:17]=[C:18]([C:22]([O:24][CH2:25][CH3:26])=[O:23])[N:19]([CH3:21])[CH:20]=1>C1COCC1>[CH3:21][N:19]1[CH:20]=[C:16]([NH:15][C:11]([NH:10][C:7]2[CH:6]=[CH:5][C:4]([O:3][C:2]([F:13])([F:14])[F:1])=[CH:9][CH:8]=2)=[O:12])[N:17]=[C:18]1[C:22]([O:24][CH2:25][CH3:26])=[O:23]

参加物

4

反応物 2

HCID 92298p-(Trifluoromethoxy)phenyl isocyanateHCID 7006687ethyl 4-amino-1-methyl-1H-imidazole-2-carboxylate

生成物 1

HCID 59421902Ethyl 1-methyl-4-[({[4-(trifluoromethoxy)phenyl]amino}carbonyl)amino]-1H-imidazole-2-carboxylate

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Under argon, 1.46 g (7.21 mmol) of 4-(trifluoromethoxy)phenyl isocyanate are added to 1.22 g (3.61 mmol) of ethyl 4-amino-1-methyl-1H-imidazole-2-carboxylate (synthesis in analogy to Example 4A step 3, or also according to Tetrahedron Lett. 2003, 44, 1607 and the literature cited therein) in 50 ml of THF, and the mixture is stirred at room temperature overnight. The reaction mixture is filtered and the filtrate is concentrated in vacuo and purified chromatographically.

後処理

  1. customsynthesis in analogy to Example 4A step 3
  2. filtrationThe reaction mixture is filtered
  3. concentrationthe filtrate is concentrated in vacuo
  4. custompurified chromatographically

出典と根拠

ORDレコード
ord-721dd9feeb6843cf82e5f636be6397c1
出典データセット
uspto-grants-2011_04
特許番号
US07919489B2

反応ノート

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