Dimethylamine → HCID 17848809、化合物

HRID 1766002ノート

反応式

HRID 1766002 の反応式
[CH3:1][NH:2][CH3:3].Cl[CH2:5][CH2:6][C:7]([C:9]1[CH:10]=[C:11]2[C:16](=[CH:17][CH:18]=1)[N:15]([C:19]([O:21][CH2:22][CH3:23])=[O:20])[CH2:14][CH2:13][CH2:12]2)=[O:8]>ClCCl>[CH3:1][N:2]([CH3:3])[CH2:5][CH2:6][C:7]([C:9]1[CH:10]=[C:11]2[C:16](=[CH:17][CH:18]=1)[N:15]([C:19]([O:21][CH2:22][CH3:23])=[O:20])[CH2:14][CH2:13][CH2:12]2)=[O:8]

参加物

4

反応物 2

HCID 674DimethylamineHCID 17848929HCID 17848929、化合物

生成物 1

HCID 17848809HCID 17848809、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

50% Aqueous dimethylamine (51 mL) was added to a solution of ethyl 6-(3-chloropropanoyl)-3,4-dihydro-1(2H)-quinoline carboxylate (15.0 g, 50.7 mmol) obtained in Reference Example 1 in dichloromethane at room temperature and then stirred for 2 hours. The reaction solution was separated, and the organic layer was washed with a saturated saline solution and dried over anhydrous sodium sulfate, and the solvent was distilled away under reduced pressure. The resultant residues were purified by alumina column chromatography (developing solvent; hexane:ethyl acetate=1:1), whereby the title compound (16.3 g) was obtained as pale yellow matter.

後処理

  1. customThe reaction solution was separated
  2. washthe organic layer was washed with a saturated saline solution
  3. dry with materialdried over anhydrous sodium sulfate
  4. distillationthe solvent was distilled away under reduced pressure
  5. customThe resultant residues were purified by alumina column chromatography (developing solvent; hexane:ethyl acetate=1:1), whereby the title compound (16.3 g)
  6. customwas obtained as pale yellow matter

出典と根拠

ORDレコード
ord-46d293a158da459d867420267f806269
出典データセット
uspto-grants-2007_06
特許番号
US07229986B2

反応ノート

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