Diethyl (ethoxymethylene)malonate → HCID 21192526、化合物

HRID 1067957ノート

反応式

HRID 1067957 の反応式
[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

参加物

4

反応物 2

HCID 6871Diethyl (ethoxymethylene)malonateHCID 21192542HCID 21192542、化合物

生成物 1

HCID 21192526HCID 21192526、化合物

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

反応条件

温度
145 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-068f9a7f45b741cd987ab3ff890bbff2
出典データセット
uspto-grants-2001_06
特許番号
US06248739B1

反応ノート

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