Hydrochloric Acid → HCID 12751826、化合物

HRID 2057449ノート

反応式

HRID 2057449 の反応式
[OH:1][C:2]1[CH:3]=[CH:4][C:5]([O:13][CH2:14][CH:15]([OH:22])[CH2:16][NH:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[C:6]2[C:11]=1[NH:10][C:9](=[O:12])[CH2:8][CH2:7]2.[OH-].[Na+].[C:25]([Cl:28])(=[O:27])[CH3:26].Cl>CC(C)=O>[ClH:28].[C:25]([O:1][C:2]1[CH:3]=[CH:4][C:5]([O:13][CH2:14][CH:15]([OH:22])[CH2:16][NH:17][C:18]([CH3:19])([CH3:21])[CH3:20])=[C:6]2[C:11]=1[NH:10][C:9](=[O:12])[CH2:8][CH2:7]2)(=[O:27])[CH3:26]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 6367Acetyl chlorideHCID 14798Sodium HydroxideHCID 1246888-Hydroxycarteolol

生成物 1

HCID 12751826HCID 12751826、化合物収率 45.5%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒2 回

実験手順

0.7 g of 8-hydroxy-5-(3-t-butylamino-2-hydroxypropoxy)-3,4-dihydrocarbostyril was suspended in 20 ml of acetone, and 3.0 ml of 1 N NaOH was added to the suspension to form a homogeneous solution. 0.2 g of acetyl chloride dissolved in a small amount of acetone was added dropwise to the solution under ice-cooling and stirring. After the mixture was allowed to stand under ice-cooling for 30 minutes, 2 ml of 1 N hydrochloric acid was added to the mixture, and the solvent evaporated under reduced pressure. The residue was purified by silica gel column chromatography using chloroform:methanol (8:1 by volume) as an eluent. The solvent was evaporated, and the residue was recrystallized from methanol-diethyl ether to obtain 0.4 g of 8-acetoxy-5-(3-t-butylamino-2-hydroxypropoxy)-3,4-dihydrocarbostyril hydrochloride as colorless flake-like crystals having a melting point of 247°-248° C. (with decomposition).

後処理

  1. customto form a homogeneous solution
  2. additionwas added dropwise to the solution under ice-
  3. temperaturecooling
  4. temperaturecooling for 30 minutes
  5. customthe solvent evaporated under reduced pressure
  6. customThe residue was purified by silica gel column chromatography
  7. customThe solvent was evaporated
  8. customthe residue was recrystallized from methanol-diethyl ether

出典と根拠

ORDレコード
ord-f749d0e0d0a440b492324a4f227a5efa
出典データセット
uspto-grants-1980_07
特許番号
US04210753

反応ノート

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