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

HRID 2277415ノート

反応式

HRID 2277415 の反応式
[CH2:1]([O:3][C:4]([C:6]1[N:7]([CH3:12])[CH:8]=[C:9]([NH2:11])[N:10]=1)=[O:5])[CH3:2].[F:13][C:14]([F:26])([F:25])[O:15][C:16]1[CH:21]=[CH:20][C:19]([N:22]=[C:23]=[O:24])=[CH:18][CH:17]=1>C1COCC1>[CH2:1]([O:3][C:4]([C:6]1[N:7]([CH3:12])[CH:8]=[C:9]([NH:11][C:23]([NH:22][C:19]2[CH:20]=[CH:21][C:16]([O:15][C:14]([F:13])([F:25])[F:26])=[CH:17][CH:18]=2)=[O:24])[N:10]=1)=[O:5])[CH3:2]

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

1.22 g (3.61 mmol) of 4-amino-1-methyl-1H-imidazole-2-carboxylic acid ethyl ester (synthesis analogous to Example 1A, Stage 3, or else according to Tetrahedron Lett. 2003, 44, 1607 and literature cited there) is mixed in 50 ml of THF under argon with 1.46 g (7.21 mmol) of 4-(trifluoromethoxy)phenylisocyanate and stirred overnight at room temperature. The reaction mixture is filtered, the filtrate is concentrated by evaporation in a vacuum, and it is purified chromatographically.

後処理

  1. filtrationThe reaction mixture is filtered
  2. concentrationthe filtrate is concentrated by evaporation in a vacuum, and it
  3. customis purified chromatographically

出典と根拠

ORDレコード
ord-d89ace771daa4b23ae15d87c3b5ce8b0
出典データセット
uspto-grants-2015_09
特許番号
US09133165B2

反応ノート

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