Diethylamine → N,N-diethylthiophene-3-carboxamide

HRID 2410242ノート

反応式

HRID 2410242 の反応式
[S:1]1[CH:5]=[CH:4][C:3]([C:6](Cl)=[O:7])=[CH:2]1.[CH2:9]([NH:11][CH2:12][CH3:13])[CH3:10]>C(Cl)Cl>[CH2:9]([N:11]([CH2:12][CH3:13])[C:6]([C:3]1[CH:4]=[CH:5][S:1][CH:2]=1)=[O:7])[CH3:10]

参加物

4

反応物 2

HCID 8021DiethylamineHCID 27763773-Thenoyl chloride

生成物 1

HCID 11389776N,N-diethylthiophene-3-carboxamide収率 91%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

Thiophene-3-carbonyl chloride was dissolved in methylene chloride (100 mL) and added to a mixture of diethylamine (43.8 g, 0.6 mol) and methylene chloride (100 mL) placed in an ice bath. Following the addition, the ice bath was removed and the resulting reaction mixture stirred at room temperature over a period of 4 h. The reaction mixture was washed several times with water and the organic layer dried over anhydrous magnesium sulfate and concentrated. Vacuum distillation of the crude residue afforded the title compound as a light yellow oil (yield: 91%): GC-Ms: 183; 1H NMR (300 MHz, CDCl3, ppm) δ: 7.36(d, 1H), 7.22-7.19(m, 1H), 7.08-7.06(m, 1H).

後処理

  1. customplaced in an ice bath
  2. additionthe addition
  3. customthe ice bath was removed
  4. customthe resulting reaction mixture
  5. washThe reaction mixture was washed several times with water
  6. dry with materialthe organic layer dried over anhydrous magnesium sulfate
  7. concentrationconcentrated
  8. distillationVacuum distillation of the crude residue

出典と根拠

ORDレコード
ord-6e90c2b556fa42a282c9985c750d8959
出典データセット
uspto-grants-2014_08
特許番号
US08816035B2

反応ノート

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