Triethylamine → 3-[2-[4-(2-Methoxyphenyl)-1-piperazinyl]ethyl]-2,4(1H,3H)-quinazolinedione

HRID 483232

反応式

HRID 483232 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[N:9]1[CH2:14][CH2:13][N:12]([CH2:15][CH:16]([NH2:26])C(=O)C2C=CC=CC=2N)[CH2:11][CH2:10]1.C([N:29]([CH2:32][CH3:33])CC)C.ClC([O:37][C:38](Cl)(Cl)Cl)=O.[C:42](=[O:45])([O-])O.[Na+]>C(Cl)Cl>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[N:9]1[CH2:10][CH2:11][N:12]([CH2:15][CH2:16][N:26]2[C:42](=[O:45])[C:33]3[C:32](=[CH:8][CH:3]=[CH:4][CH:5]=3)[NH:29][C:38]2=[O:37])[CH2:13][CH2:14]1

参加物

6

反応物 4

HCID 8471TriethylamineHCID 10426DiphosgeneHCID 516892Sodium BicarbonateHCID 571547151-(2-Methoxyphenyl)-4-[2-(2-aminobenzoyl)-aminoethyl]piperazine

生成物 1

HCID 1220653-[2-[4-(2-Methoxyphenyl)-1-piperazinyl]ethyl]-2,4(1H,3H)-quinazolinedione

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

A mixture of 1-(2-methoxyphenyl)-4-[2-(2-aminobenzoyl)-aminoethyl]piperazine (3.54 g) and triethylamine (2.2 g) was dissolved in methylene chloride (50 ml), and the resulting solution was added dropwise to a solution of trichloromethyl chloroformate (0.989 g) in methylene chloride (20 ml) under stirring at between -5° and 5° C. Then, the mixture was gradually heated to room temperature at which it was held for 1 to 2 hours to effect reaction. After completion of the reaction, saturated aqueous sodium hydrogencarbonate was added to the reaction mixture and the resulting mixture was extracted with methylene chloride, the methylene chloride layer was washed with water twice and dried on anhydrous magnesium sulfate. The solvent was concentrated under vacuum and isopropanol was added to the residue to give 2.28 g of crystalline 3-[2-[4-(2-methoxyphenyl)-1-piperazinyl]-ethyl]-2,4-(1H,3H)quinazolinedione having a melting point of 217°-218° C. (recrystallized from chloroform-ether).

後処理

  1. customreaction
  2. additionwas added to the reaction mixture
  3. extractionthe resulting mixture was extracted with methylene chloride
  4. washthe methylene chloride layer was washed with water twice
  5. dry with materialdried on anhydrous magnesium sulfate
  6. concentrationThe solvent was concentrated under vacuum and isopropanol
  7. additionwas added to the residue

出典と根拠

ORDレコード
ord-62a9f048b6a045bdbc15ff6899d92e73
出典データセット
uspto-grants-1986_03
特許番号
US04578465

関連ノート

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