Diethyl (ethoxymethylene)malonate → 10-bromo-5-ethoxycarbonyl-2-methoxy-4H-pyrido [3,2,1-jk]carbazole-4-one

HRID 1530981ノート

反応式

HRID 1530981 の反応式
[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[NH:6][C:7]3[C:12]([C:13]=2[CH:14]=1)=[CH:11][C:10]([O:15][CH3:16])=[CH:9][CH:8]=3.C([O:19][CH:20]=[C:21]([C:27](OCC)=O)[C:22]([O:24][CH2:25][CH3:26])=[O:23])C>C1(C)C(C)=CC=CC=1>[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[N:6]3[CH:27]=[C:21]([C:22]([O:24][CH2:25][CH3:26])=[O:23])[C:20](=[O:19])[C:8]4[CH:9]=[C:10]([O:15][CH3:16])[CH:11]=[C:12]([C:13]=2[CH:14]=1)[C:7]3=4

参加物

4

反応物 2

HCID 6871Diethyl (ethoxymethylene)malonateHCID 15886922HCID 15886922、化合物

生成物 1

HCID 2125285710-bromo-5-ethoxycarbonyl-2-methoxy-4H-pyrido [3,2,1-jk]carbazole-4-one収率 50%

試薬・触媒・溶媒 1

HCID 7237O-Xylene溶媒

実験手順

3-bromo-6-methoxycarbazole (2.5 g) produced in Example 1, step 1 and diethyl ethoxymethylenemalonate (9.16 ml) were dissolved in xylene, and the solution was heated under reflux in an argon atmosphere for 120 hours, and allowed to cool. The solvent was evaporated under reduced pressure and the residue was purified by silica gel column chromatography (eluent: chloroform) to obtain the title compound (2 g, 50%).

後処理

  1. temperaturethe solution was heated
  2. temperatureunder reflux in an argon atmosphere for 120 hours
  3. temperatureto cool
  4. customThe solvent was evaporated under reduced pressure
  5. customthe residue was purified by silica gel column chromatography (eluent: chloroform)

出典と根拠

ORDレコード
ord-789a2fc874384b20a9791083ef833f30
出典データセット
uspto-grants-2001_03
特許番号
US06197768B1

反応ノート

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