Methyl 2,2,2-trichloroacetimidate → HCID 178497356、化合物

HRID 18512

反応式

HRID 18512 の反応式
[CH3:1][O:2][C:3](=[O:12])[C:4]1[CH:9]=[CH:8][C:7]([NH2:10])=[C:6]([NH2:11])[CH:5]=1.CO[C:15](=N)[C:16]([Cl:19])([Cl:18])[Cl:17]>C(O)(=O)C.C1(C)C=CC=CC=1>[CH3:1][O:2][C:3]([C:4]1[CH:9]=[CH:8][C:7]2[NH:10][C:15]([C:16]([Cl:19])([Cl:18])[Cl:17])=[N:11][C:6]=2[CH:5]=1)=[O:12]

参加物

5

反応物 2

HCID 100479Methyl 2,2,2-trichloroacetimidateHCID 1355243,5-Diamino-2-methylbenzoic acid

生成物 1

HCID 178497356HCID 178497356、化合物

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 1140Toluene溶媒

実験手順

2.00 g (12.0 mmol) Methyl-3,4-diamino-benzoate were dissolved in 50 mL concentrated acetic acid. Then 2.09 mL (1.4 equiv.) methyl-2,2,2-trichloroacetimidate were added slowly and the resulting mixture was stirred at room temperature for 2 h. The mixture was diluted with 100 mL toluene and the solvent was removed under reduced pressure. The residue was taken up in dichloromethane and washed once with a saturated NaHCO3-solution and once with brine. The organic layer was dried over MgSO4 and the solvent was removed under reduced pressure to give pure methyl-2-trichloromethyl-1H-benzoimidazole-5-carboxylate as a light brown amorphous solid. Yield: 3.64 g MS (ES+): m/e=293, chloro pattern.

後処理

  1. customthe solvent was removed under reduced pressure
  2. washwashed once with a saturated NaHCO3-solution and once with brine
  3. dry with materialThe organic layer was dried over MgSO4
  4. customthe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-adba86b5f34648e9b32436231fe51488
出典データセット
uspto-grants-2010_06
特許番号
US07741341B2

関連ノート

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