Sodium Chloride → 1-methyl-6-[3-(N-cyclohexyl-N-methylaminocarbonyl)propoxy]-3,4-dihydrocarbostyril

HRID 1154955ノート

反応式

HRID 1154955 の反応式
[CH3:1][N:2]1[C:12]2[C:7](=[CH:8][C:9]([OH:13])=[CH:10][CH:11]=2)[CH2:6][CH2:5][C:3]1=[O:4].[OH-].[K+].[I-].[Na+].[CH3:18][N:19]([CH:26]1[CH2:31][CH2:30][CH2:29][CH2:28][CH2:27]1)[C:20](=[O:25])[CH2:21][CH2:22][CH2:23]Cl.[Na+].[Cl-]>CS(C)=O>[CH3:1][N:2]1[C:12]2[C:7](=[CH:8][C:9]([O:13][CH2:23][CH2:22][CH2:21][C:20]([N:19]([CH:26]3[CH2:27][CH2:28][CH2:29][CH2:30][CH2:31]3)[CH3:18])=[O:25])=[CH:10][CH:11]=2)[CH2:6][CH2:5][C:3]1=[O:4]

参加物

7

反応物 5

HCID 5234Sodium ChlorideHCID 5238Sodium IodideHCID 14797Potassium HydroxideHCID 132082974-Chloro-N-cyclohexyl-N-methylbutanamideHCID 219318286-Hydroxy-1-methyl-3,4-dihydroquinolin-2(1H)-one

生成物 1

HCID 155729261-methyl-6-[3-(N-cyclohexyl-N-methylaminocarbonyl)propoxy]-3,4-dihydrocarbostyril

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

3.4 Grams of 1-methyl-6-hydroxy-3,4-dihydrocarbostyril, 0.9 g of potassium hydroxide, 3.2 g of sodium iodide and 5.0 g of N-methyl-N-(4-chlorobutyryl)-cyclohexylamine are added to 50 ml of dimethylsulfoxide and agitated at 70° to 80° C. for 4.5 hours. After the reaction, the reaction solution is poured into 400 ml of saturated NaCl solution and the precipitated crystals are filtered out and washed with water. The resultant crude crystals are recrystallized from ligroin to obtain 3.1 g of 1-methyl-6-[3-(N-cyclohexyl-N-methylaminocarbonyl)propoxy]-3,4-dihydrocarbostyril in the form of colorless needle-like crystals with melting point of 104.5°-106.5° C.

後処理

  1. customAfter the reaction
  2. filtrationthe precipitated crystals are filtered out
  3. washwashed with water
  4. customThe resultant crude crystals are recrystallized from ligroin

出典と根拠

ORDレコード
ord-aa3ec323e8884819b08c252bec27136e
出典データセット
uspto-grants-1981_11
特許番号
US04298739

反応ノート

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