Hydrochloric Acid → HCID 20469098, 화합물

HRID 1388937노트

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HRID 1388937 반응식
[CH3:1][N:2]1[CH:6]=[CH:5][CH:4]=[C:3]1[CH3:7].[CH3:8][N:9]1[C:13]([C:14](Cl)=[O:15])=[C:12]([CH3:17])[CH:11]=[C:10]1[CH2:18][C:19]([O:21][C:22]([CH3:25])([CH3:24])[CH3:23])=[O:20].Cl[Sn](Cl)(Cl)Cl.Cl>C(Cl)Cl>[CH3:8][N:9]1[C:13]([C:14]([C:6]2[N:2]([CH3:1])[C:3]([CH3:7])=[CH:4][CH:5]=2)=[O:15])=[C:12]([CH3:17])[CH:11]=[C:10]1[CH2:18][C:19]([O:21][C:22]([CH3:25])([CH3:24])[CH3:23])=[O:20]

참가 물질

6

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HCID 313Hydrochloric AcidHCID 24287Tin tetrachlorideHCID 38261981,2-Dimethyl-1H-pyrroleHCID 86739290HCID 86739290, 화합물

생성물 1

HCID 20469098HCID 20469098, 화합물수율 50%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

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온도
0 °C

실험 절차

Ten mmole (0.95 g) of 1,2-dimethyl-pyrrole and an equivalent amount of t-butyl 1,4-dimethyl-5-chlorocarbonyl-2-pyrrole acetate were dissolved in 10 ml of methylene chloride and stirred at 0° C. under nitrogen atmosphere. Three grams (12 mmole) of SnCl4 in 10 ml methylene chloride was added dropwise and the resulting mixture was stirred at room temperature for three hours followed by pouring into 25 ml 6 N HCl at 0° C. with vigorous stirring. The resulting suspension was extracted three times with 20 ml portions of methylene chloride. The crude extract was column chromatographed and crystallized from ether/hexane to give 1.6 g (50%) of t-butyl 1,4-dimethyl-5-(1,5-dimethylpyrrol-2-oyl)pyrrole-2-acetate.

후처리

  1. stirringthe resulting mixture was stirred at room temperature for three hours
  2. extractionThe resulting suspension was extracted three times with 20 ml portions of methylene chloride
  3. extractionThe crude extract
  4. customchromatographed
  5. customcrystallized from ether/hexane

출처 및 근거

ORD 기록
ord-16040c41e5e044e198b4460cbf1a3174
출처 데이터셋
uspto-grants-1984_02
특허 번호
US04434175

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