Hydrochloric Acid → HCID 20469098、化合物

HRID 1388937ノート

反応式

HRID 1388937 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

HCID 20469098HCID 20469098、化合物収率 50%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

反応条件

温度
0 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-16040c41e5e044e198b4460cbf1a3174
出典データセット
uspto-grants-1984_02
特許番号
US04434175

反応ノート

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