Potassium Carbonate → HCID 12763962, 화합물

HRID 616705노트

반응식

HRID 616705 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 12763962HCID 12763962, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-88cc3fadfea24e24b29f90dc3851a99b
출처 데이터셋
uspto-grants-1978_02
특허 번호
US04075343

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