Bromine → Methyl 5-bromo-2-({[(trichloroacetyl)amino]carbonyl}amino)thiophene-3-carboxylate

HRID 30345

反応式

HRID 30345 の反応式
[Cl:1][C:2]([Cl:19])([Cl:18])[C:3]([NH:5][C:6]([NH:8][C:9]1[S:10][CH:11]=[CH:12][C:13]=1[C:14]([O:16][CH3:17])=[O:15])=[O:7])=[O:4].[Br:20]Br>C(O)(=O)C>[Br:20][C:11]1[S:10][C:9]([NH:8][C:6]([NH:5][C:3](=[O:4])[C:2]([Cl:1])([Cl:18])[Cl:19])=[O:7])=[C:13]([C:14]([O:16][CH3:17])=[O:15])[CH:12]=1

参加物

4

反応物 2

HCID 24408BromineHCID 59789494Methyl 2-({[(trichloroacetyl)amino]carbonyl}amino)thiophene-3-carboxylate

生成物 1

HCID 59789485Methyl 5-bromo-2-({[(trichloroacetyl)amino]carbonyl}amino)thiophene-3-carboxylate

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒2 回

実験手順

To a stirred solution of methyl 2-({[(trichloroacetyl)amino]carbonyl}amino)thiophene-3-carboxylate (1 eq) in glacial acetic acid (20 mL) was added a solution of bromine (1.3 eq) in glacial acetic acid (5 mL) slowly over a period of 5 min. After the addition was complete, the resulting dark solution was stirred for 30 mins at RT. The solvent was evaporated under vaccum and the residue was triturated with H2O. The title compound was obtained by filtration (99%) as an off-white solid. The product was used in the next step without any further purification after drying for 2 days under P2O5. LC/MS (ES, M+H=425).

後処理

  1. additionAfter the addition
  2. customThe solvent was evaporated under vaccum
  3. customthe residue was triturated with H2O

出典と根拠

ORDレコード
ord-ef5a843594ce4bdbbd44b4fce50222a8
出典データセット
uspto-grants-2008_09
特許番号
US07423061B2

関連ノート

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