Triethylamine → 4-Bromothiophene-2-carboxamide

HRID 2206042노트

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HRID 2206042 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 128360674-Bromothiophene-2-carboxamide

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-0f1ba51f32a04372a29cf5d9aeac3bbb
출처 데이터셋
uspto-grants-2016_06
특허 번호
US09371320B2

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