Sodium hydride → HCID 20034517, 화합물

HRID 231076

반응식

HRID 231076 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 20034517HCID 20034517, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-9393e4b407154a35ba3fa509557bbd05
출처 데이터셋
uspto-grants-1989_07
특허 번호
US04845099

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