Ethylamine → N-ethylthiophene-2-carboxamide

HRID 368665노트

반응식

HRID 368665 반응식
[S:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[C:6](Cl)=[O:7].[CH2:9]([NH2:11])[CH3:10]>C(Cl)Cl.O>[CH2:9]([NH:11][C:6]([C:2]1[S:1][CH:5]=[CH:4][CH:3]=1)=[O:7])[CH3:10]

참가 물질

5

반응물 2

HCID 6341EthylamineHCID 789282-Thiophenecarbonyl chloride

생성물 1

HCID 5151566N-ethylthiophene-2-carboxamide수율 83.1%

시약·촉매·용매 2

HCID 962Water용매2회HCID 6344Dichloromethane용매

실험 절차

A solution of 2-thiophenecarboxylic acid chloride (7.3 g, 50 mmol) in 30 mL CH2Cl2 was added to 70% ethylamine in water (11 g) at -5° C. and the resulting solution was stirred at RT for 18 h. After that, water was added. The organic layer was separated, washed with water, brine, dried and concentrated. Purification of the residue by flash chromatography with 25% ethyl acetate-hexane gave 6.4 g (83.1% yield) of N-ethyl-2-thiophenecarboxamide as a white solid, m.p. 75-78° C.

후처리

  1. customThe organic layer was separated
  2. washwashed with water, brine
  3. customdried
  4. concentrationconcentrated
  5. customPurification of the residue by flash chromatography with 25% ethyl acetate-hexane

출처 및 근거

ORD 기록
ord-55754e3af81c4d708e8a8732e5006c57
출처 데이터셋
uspto-grants-2000_10
특허 번호
US06133252

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