2,5-Dichlorobenzenesulfonyl chloride → 2,4-Dimethyl-1-[3-(2,5-dichlorbenzenesulphonamido)propyl]-pyrrolidine

HRID 1731540ノート

反応式

HRID 1731540 の反応式
[CH3:1][CH:2]1[CH2:6][CH:5]([CH3:7])[CH2:4][N:3]1[CH2:8][CH2:9][CH2:10][NH2:11].[Cl:12][C:13]1[CH:18]=[CH:17][C:16]([Cl:19])=[CH:15][C:14]=1[S:20](Cl)(=[O:22])=[O:21]>C1C=CC=CC=1>[CH3:1][CH:2]1[CH2:6][CH:5]([CH3:7])[CH2:4][N:3]1[CH2:8][CH2:9][CH2:10][NH:11][S:20]([C:14]1[CH:15]=[C:16]([Cl:19])[CH:17]=[CH:18][C:13]=1[Cl:12])(=[O:22])=[O:21]

参加物

4

反応物 2

HCID 794012,5-Dichlorobenzenesulfonyl chlorideHCID 202277352,4-Dimethyl-1-(3-aminopropyl)pyrrolidine

生成物 1

HCID 202277722,4-Dimethyl-1-[3-(2,5-dichlorbenzenesulphonamido)propyl]-pyrrolidine収率 67%

試薬・触媒・溶媒 1

HCID 241Benzene溶媒2 回

実験手順

2,4-Dimethyl-1-(3-aminopropyl)pyrrolidine in (4.7 g, 0.03 mol) benzene (30 ml) was added dropwise at room temperature to a solution of 2,5-dichlorobenzenesulphonylchloride (7.3 g, 0.03 ml) in benzene (100 ml). Thereafter, the mixture was stirred for 4 days at room temperature until the reaction was complete. Finally, the reaction product was obtained as a viscous, oily paste. The benzene mother liquor was decanted. The residue was dissolved in water, the solution was adjusted to pH 9.8 with 10% NaOH and extractes with petroleum ether (40°-60°) (4×100 ml). The combined extracts were dried over Na2SO4 and evaporated. The residue (5 g) was recrystallised twice from 100 ml petroleum ether to yield the product (3.7 g as white needles), m.p. 65°-67° C. Yield=67% of theoretical

後処理

  1. customFinally, the reaction product was obtained as a viscous, oily paste
  2. customThe benzene mother liquor was decanted
  3. dissolutionThe residue was dissolved in water
  4. customwas adjusted to pH 9.8 with 10% NaOH and extractes with petroleum ether (40°-60°) (4×100 ml)
  5. dry with materialThe combined extracts were dried over Na2SO4
  6. customevaporated
  7. customThe residue (5 g) was recrystallised twice from 100 ml petroleum ether
  8. customto yield the product (3.7 g as white needles), m.p. 65°-67° C

出典と根拠

ORDレコード
ord-3e6134f02812472faa64f0e57b1f1f9e
出典データセット
uspto-grants-1986_11
特許番号
US04622331

反応ノート

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