Dimethylamine → HCID 17848809, 화합물

HRID 1766002노트

반응식

HRID 1766002 반응식
[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]

참가 물질

4

반응물 2

HCID 674DimethylamineHCID 17848929HCID 17848929, 화합물

생성물 1

HCID 17848809HCID 17848809, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-46d293a158da459d867420267f806269
출처 데이터셋
uspto-grants-2007_06
특허 번호
US07229986B2

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