Triethylamine → HCID 57467435, 화합물

HRID 1890778노트

반응식

HRID 1890778 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 57467435HCID 57467435, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-d06c4abb71ac42d49bfeee6ffa365b06
출처 데이터셋
uspto-grants-2013_08
특허 번호
US08507493B2

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