Sodium hydride → HCID 20034517、化合物

HRID 231076ノート

反応式

HRID 231076 の反応式
[H-].[Na+].[OH:3][C:4]1[CH:5]=[CH:6][CH:7]=[C:8]2[C:13]=1[N:12]([C:14](=[O:21])[C:15]1[CH:20]=[CH:19][CH:18]=[N:17][CH:16]=1)[CH2:11][CH2:10][CH2:9]2.[Cl:22][CH2:23][CH2:24][CH2:25][N:26]1[CH2:31][CH2:30][N:29]([C:32]2[CH:37]=[CH:36][CH:35]=[CH:34][C:33]=2[O:38][CH3:39])[CH2:28][CH2:27]1>CN(C)C=O>[ClH:22].[ClH:22].[ClH:22].[CH3:39][O:38][C:33]1[CH:34]=[CH:35][CH:36]=[CH:37][C:32]=1[N:29]1[CH2:28][CH2:27][N:26]([CH2:25][CH2:24][CH2:23][O:3][C:4]2[CH:5]=[CH:6][CH:7]=[C:8]3[C:13]=2[N:12]([C:14](=[O:21])[C:15]2[CH:20]=[CH:19][CH:18]=[N:17][CH:16]=2)[CH2:11][CH2:10][CH2:9]3)[CH2:31][CH2:30]1

参加物

5

反応物 3

HCID 24758Sodium hydrideHCID 6226691-(3-Chloropropyl)-4-(2-methoxyphenyl)piperazineHCID 30187391,2,3,4-Tetrahydro-1-(3-pyridylcarbonyl)quinolin-8-ol

生成物 1

HCID 20034517HCID 20034517、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

0.53 (11.0 mmol) of a 50% strength sodium hydride dispersion is introduced in portions into a solution of 2.54 g (10.0 mmol) of 8-hydroxy-1-nicotinoyl-1,2,3,4-tetrahydroquinoline in 20 ml of anhydrous dimethylformamide and the mixture is subsequently stirred at 40°-50° C. for 30 minutes. After cooling to room temperature, a solution of 4.03 g (15.0 mmol) of 1-(3-chloropropyl)-4-(2-methoxyphenyl)piperazine in 20 ml of anhydrous dimethylformamide is added dropwise and the mixture is subsequently stirred at room temperature for 16 hours. The reaction solution is poured onto 150 ml of ice-water and extracted with methylene chloride and the extracts are washed several times with water, dried and concentrated. The crude product is further purified by column chromatography on silica gel (mobile phase toluene:ethanol 9:1) and converted into the dihydrochloride as described under Example 2(a). The product thus obtained is identical to the product described under 2(a).

後処理

  1. stirringthe mixture is subsequently stirred at room temperature for 16 hours
  2. extractionextracted with methylene chloride
  3. washthe extracts are washed several times with water
  4. customdried
  5. concentrationconcentrated
  6. customThe crude product is further purified by column chromatography on silica gel (mobile phase toluene:ethanol 9:1)
  7. customThe product thus obtained

出典と根拠

ORDレコード
ord-9393e4b407154a35ba3fa509557bbd05
出典データセット
uspto-grants-1989_07
特許番号
US04845099

反応ノート

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