Triethylamine → HCID 57467435、化合物

HRID 1890778ノート

反応式

HRID 1890778 の反応式
[CH3:1][C:2]([O:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)([CH3:6])[C:3]([NH2:5])=O.C(N(CC)CC)C.FC(F)(F)C(OC(=O)C(F)(F)F)=O>C(Cl)Cl>[CH3:6][C:2]([O:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)([CH3:1])[C:3]#[N:5]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 9845Trifluoroacetic anhydrideHCID 123215122-Methyl-2-phenoxypropanamide

生成物 1

HCID 57467435HCID 57467435、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 2-methyl-2-phenoxypropanamide from Step C (0.01 mol) in dry CH2Cl2 (50 mL) and triethylamine (3.03 g, 0.03 mol) at 0° C. was added trifluoroacetic anhydride (3.15 g, 0.015 mol). After the addition was complete, the solution was allowed to warm to room temperature and stirring was continued at ambient temperature overnight. The reaction mixture was then refluxed for 3 hours. After cooling to room temperature and dilution with CH2Cl2 (100 mL), the solution was washed with saturated aqueous NaHCO3 (50 mL×3), water, and brine and dried over sodium sulfated. Evaporation gave the titled compound. 1H NMR (400 MHz, CDCl3) δ ppm 7.32˜7.36 (m, 2H), 7.14˜7.20 (m, 3H), 1.71 (s, 6H).

後処理

  1. additionAfter the addition
  2. temperatureThe reaction mixture was then refluxed for 3 hours
  3. temperatureAfter cooling to room temperature
  4. washdilution with CH2Cl2 (100 mL), the solution was washed with saturated aqueous NaHCO3 (50 mL×3), water, and brine
  5. dry with materialdried over sodium
  6. customEvaporation

出典と根拠

ORDレコード
ord-d06c4abb71ac42d49bfeee6ffa365b06
出典データセット
uspto-grants-2013_08
特許番号
US08507493B2

反応ノート

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