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

HRID 47112

反応式

HRID 47112 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-866b4918b68a46828ad29f644d56bd5a
出典データセット
uspto-grants-1979_11
特許番号
US04176184

関連ノート

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