Potassium Carbonate → 2,7,7-Trimethyl-5-(2-diethylamino-ethyl)-5H,7H-imidazo[4,5-h]isoquinoline-4,6-dione hydrochloride

HRID 47112

반응식

HRID 47112 반응식
[CH3:1][C:2]1[N:18]=[C:5]2[C:6](=[O:17])[CH2:7][CH:8]3[C:13]([CH:12]=[N:11][C:10]([CH3:15])([CH3:14])[C:9]3=[O:16])=[C:4]2[N:3]=1.Cl.[CH2:20]([N:22]([CH2:25][CH2:26][Cl:27])[CH2:23][CH3:24])[CH3:21].C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[ClH:27].[CH3:1][C:2]1[N:18]=[C:5]2[C:6](=[O:17])[CH:7]([CH2:21][CH2:20][N:22]([CH2:25][CH3:26])[CH2:23][CH3:24])[CH:8]3[C:13]([CH:12]=[N:11][C:10]([CH3:14])([CH3:15])[C:9]3=[O:16])=[C:4]2[N:3]=1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 133631-Chloro-2-(diethylamine)ethane hydrochlorideHCID 706107882,7,7-trimethyl-5H,7H-imidazo[4,5-h]isoquinoline-4,6-dione

생성물 1

HCID 706111972,7,7-Trimethyl-5-(2-diethylamino-ethyl)-5H,7H-imidazo[4,5-h]isoquinoline-4,6-dione hydrochloride

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

4.2 gm of 2,7,7-trimethyl-5H,7H-imidazo[4,5-h]isoquinoline-4,6-dione were dissolved in 100 ml of dimethylformamide, and the solution was admixed with 3.4 gm of diethylamino ethyl chloride hydrochloride and 4.1 gm of potassium carbonate. The mixture was refluxed for 8 hours, the solvent was distilled off in vacuo, the residue was admixed with water and extracted with chloroform. The chloroform phase was evaporated and the residue was purified on a silicagel column (eluant: chloroform/acetone 19:1). The dihydrochloride was precipitated from acetone/methanol with ethereal hydrochloric acid and recrystallized from acetone/methanol.

후처리

  1. temperatureThe mixture was refluxed for 8 hours
  2. distillationthe solvent was distilled off in vacuo
  3. extractionextracted with chloroform
  4. customThe chloroform phase was evaporated
  5. customthe residue was purified on a silicagel column (eluant: chloroform/acetone 19:1)
  6. customThe dihydrochloride was precipitated from acetone/methanol with ethereal hydrochloric acid
  7. customrecrystallized from acetone/methanol

출처 및 근거

ORD 기록
ord-866b4918b68a46828ad29f644d56bd5a
출처 데이터셋
uspto-grants-1979_11
특허 번호
US04176184

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