Diethyl (ethoxymethylene)malonate → HCID 21192526, 화합물

HRID 1067957노트

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HRID 1067957 반응식
[CH:1]1([NH:4][C:5]2[CH:10]=[CH:9][C:8]([CH2:11][N:12]3[CH2:17][CH2:16][O:15][CH2:14][CH2:13]3)=[CH:7][CH:6]=2)[CH2:3][CH2:2]1.C(O[CH:21]=[C:22]([C:28]([O:30][CH2:31][CH3:32])=[O:29])[C:23]([O:25][CH2:26][CH3:27])=[O:24])C>N1C=CC=CC=1>[CH:1]1([N:4]([CH:21]=[C:22]([C:23]([O:25][CH2:26][CH3:27])=[O:24])[C:28]([O:30][CH2:31][CH3:32])=[O:29])[C:5]2[CH:6]=[CH:7][C:8]([CH2:11][N:12]3[CH2:13][CH2:14][O:15][CH2:16][CH2:17]3)=[CH:9][CH:10]=2)[CH2:3][CH2:2]1

참가 물질

4

반응물 2

HCID 6871Diethyl (ethoxymethylene)malonateHCID 21192542HCID 21192542, 화합물

생성물 1

HCID 21192526HCID 21192526, 화합물

시약·촉매·용매 1

HCID 1049Pyridine용매

반응 조건

온도
145 °C

실험 절차

To a flask containing N-cyclopropyl-4-(4-morpholinylmethyl)aniline (0.55 g) from Preparation No. 23 is added diethyl ethoxymethylenemalonate (0.45 mL) and pyridine (0.33 mL). The flask is tightly capped and heated to 145° C. for 2 hours. The reaction is cooled to room temperature and azeotroped under reduced pressure with toluene (3×). The residue is dissolved in dichloromethane and washed with brine, dried and concentrated under reduced pressure. The residue is chromatographed on silica eluting with 2% to 6% methanol in dichloromethane. The product-containing fractions are evaporated to give 0.77 g of the title compound as an oil.

후처리

  1. customfrom Preparation No
  2. customThe flask is tightly capped
  3. temperatureThe reaction is cooled to room temperature
  4. customazeotroped under reduced pressure with toluene (3×)
  5. dissolutionThe residue is dissolved in dichloromethane
  6. washwashed with brine
  7. customdried
  8. concentrationconcentrated under reduced pressure
  9. customThe residue is chromatographed on silica eluting with 2% to 6% methanol in dichloromethane
  10. customThe product-containing fractions are evaporated

출처 및 근거

ORD 기록
ord-068f9a7f45b741cd987ab3ff890bbff2
출처 데이터셋
uspto-grants-2001_06
특허 번호
US06248739B1

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