Potassium Carbonate → HCID 12763962、化合物

HRID 616705ノート

反応式

HRID 616705 の反応式
[NH2:1][C:2]1[CH:11]=[C:10]([Cl:12])[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[N:3]=1.C(=O)([O-])[O-].[K+].[K+].Br[CH2:20][C:21](=O)[C:22]([O:24][CH2:25][CH3:26])=[O:23]>CN(C)C=O>[Cl:12][C:10]1[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[N:3]2[CH:20]=[C:21]([C:22]([O:24][CH2:25][CH3:26])=[O:23])[N:1]=[C:2]2[CH:11]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 66144Ethyl bromopyruvateHCID 140674074-Chloroquinolin-2-amine

生成物 1

HCID 12763962HCID 12763962、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To 200 ml. of N,N-dimethylformamide is added 17.9 g. (0.10 mole) of 2-amino-4-chloroquinoline and 15.2 g. (0.11 mole) potassium carbonate. To this stirred slurry is added dropwise over 20 minutes 21.5 g. (0.11 mole) of ethyl bromopyruvate and the resulting mixture stirred for two hours. The solvent is then removed in vacuo and the residue was triturated with water, extracted three times with ethyl acetate, the extracts dried over anhydrous sodium sulfate, carbon treated, filtered and the solvent evaporated to afford the title compound. Further purification is achieved by crystallization or silica gel chromatography.

後処理

  1. additionTo this stirred slurry is added dropwise over 20 minutes 21.5 g
  2. customThe solvent is then removed in vacuo
  3. customthe residue was triturated with water
  4. extractionextracted three times with ethyl acetate
  5. dry with materialthe extracts dried over anhydrous sodium sulfate, carbon
  6. additiontreated
  7. filtrationfiltered
  8. customthe solvent evaporated

出典と根拠

ORDレコード
ord-88cc3fadfea24e24b29f90dc3851a99b
出典データセット
uspto-grants-1978_02
特許番号
US04075343

反応ノート

読み込み中…