Potassium Carbonate → HCID 21958890, 화합물

HRID 1793426노트

반응식

HRID 1793426 반응식
Cl[CH2:2][CH2:3][CH2:4][N:5]1[CH2:10][CH2:9][O:8][CH2:7][CH2:6]1.[C:11]([O:22][CH2:23][CH3:24])(=[O:21])[C:12]1[CH:20]=[CH:19][C:17]([OH:18])=[C:14]([O:15][CH3:16])[CH:13]=1.C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[CH3:16][O:15][C:14]1[CH:13]=[C:12]([CH:20]=[CH:19][C:17]=1[O:18][CH2:2][CH2:3][CH2:4][N:5]1[CH2:10][CH2:9][O:8][CH2:7][CH2:6]1)[C:11]([O:22][CH2:23][CH3:24])=[O:21]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 12038Ethyl vanillateHCID 958344-(3-Chloropropyl)morpholine

생성물 1

HCID 21958890HCID 21958890, 화합물수율 100%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
80 °C

실험 절차

N-(3-Chloropropyl)morpholine (90 g, 0.55 mol) was added dropwise, over 30 minutes, to a solution of ethyl vanillate (98 g, 0.50 mol) and powdered potassium carbonate (104 g, 0.75 mol) in dimethylformamide (300 ml) at 80° C. The reaction was heated at 80° C. for 90 minutes, cooled to ambient temperature, filtered and the filtrate concentrated in vacuo. The crude product was taken up in diethyl ether (1000 ml), filtered and washed with water (2×200 ml) and brine (200 ml). Solvent evaporation in vacuo yielded ethyl 3-methoxy-4-(3-morpholinopropoxy)benzoate (161.5 g, 100% yield) as a pale yellow oil which crystallised on standing to afford a pale yellow solid:

후처리

  1. temperaturecooled to ambient temperature
  2. filtrationfiltered
  3. concentrationthe filtrate concentrated in vacuo
  4. filtrationfiltered
  5. washwashed with water (2×200 ml) and brine (200 ml)
  6. customSolvent evaporation in vacuo

출처 및 근거

ORD 기록
ord-8be430819dbb4a75bfe5bbc25789aab5
출처 데이터셋
uspto-grants-2006_07
특허 번호
US07081461B1

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