Triethylamine → 4-Bromothiophene-2-carboxamide

HRID 2206042ノート

反応式

HRID 2206042 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([C:7]([OH:9])=O)[S:5][CH:6]=1.C([N:12](CC)CC)C.CCN=C=NCCCN(C)C.Cl>C(#N)C>[Br:1][C:2]1[CH:3]=[C:4]([C:7]([NH2:12])=[O:9])[S:5][CH:6]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 6104094-Bromo-2-thiophenecarboxylic AcidHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride

生成物 1

HCID 128360674-Bromothiophene-2-carboxamide

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

To a solution of 4-bromothiophene-2-carboxylic acid (15 g), HOBt ammonium salt (16.5 g) and triethylamine (20.08 mL) in acetonitrile (250 mL) was added EDCI hydrochloride (16.87 g), and the mixture was stirred overnight. The reaction mixture was washed with saturated aqueous sodium bicarbonate solution and saturated brine, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (8.0 g).

後処理

  1. washThe reaction mixture was washed with saturated aqueous sodium bicarbonate solution and saturated brine
  2. dry with materialdried over anhydrous sodium sulfate
  3. concentrationconcentrated under reduced pressure
  4. customThe residue was purified by silica gel column chromatography (ethyl acetate/hexane)

出典と根拠

ORDレコード
ord-0f1ba51f32a04372a29cf5d9aeac3bbb
出典データセット
uspto-grants-2016_06
特許番号
US09371320B2

反応ノート

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