Dibutylamine → HCID 20505824、化合物

HRID 1390512ノート

反応式

HRID 1390512 の反応式
[CH2:1]([NH:5][CH2:6][CH2:7][CH2:8][CH3:9])[CH2:2][CH2:3][CH3:4].[Cl:10][C:11]1[C:19]([S:20](Cl)(=[O:22])=[O:21])=[CH:18][C:14]([C:15]([OH:17])=[O:16])=[CH:13][CH:12]=1>C(Cl)Cl>[Cl:10][C:11]1[C:19]([S:20](=[O:22])(=[O:21])[N:5]([CH2:6][CH2:7][CH2:8][CH3:9])[CH2:1][CH2:2][CH2:3][CH3:4])=[CH:18][C:14]([C:15]([OH:17])=[O:16])=[CH:13][CH:12]=1

参加物

4

反応物 2

HCID 8148DibutylamineHCID 756134-Chloro-3-(chlorosulphonyl)benzoic acid

生成物 1

HCID 20505824HCID 20505824、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 3.9 g. (0.03 mole) of di-n-butylamine in 15 ml. of methylene chloride is added 2.5 g. (0.01 mole) of 4-chloro-5-chlorosulfonylbenzoic acid (J. Pharm. Pharmacol., 683 (1962), and the resulting reaction mixture allowed to stir at room temperature for 3 hrs. The solvent is removed under reduced pressure and the residue partitioned between 1N sodium hydroxide and diethyl ether. The aqueous phase is separated, acidified with 12N hydrochloric acid and the precipitated solid filtered and dried, 3.0 g., m.p. 93°-96° C. Recrystallization from ether-hexane provides the pure product, 2.5 g., m.p. 94.5°-96.5° C.

後処理

  1. custom, 683 (1962), and the resulting reaction mixture
  2. customThe solvent is removed under reduced pressure
  3. customthe residue partitioned between 1N sodium hydroxide and diethyl ether
  4. customThe aqueous phase is separated
  5. filtrationthe precipitated solid filtered
  6. customdried
  7. customRecrystallization from ether-hexane
  8. customprovides the pure product, 2.5 g

出典と根拠

ORDレコード
ord-50abda334e24435f9a04cb793cde78eb
出典データセット
uspto-grants-1979_02
特許番号
US04138399

反応ノート

読み込み中…