Benzoic acid, 2-chloro-5-(chlorosulfonyl)- → HCID 20505867、化合物

HRID 355129

反応式

HRID 355129 の反応式
[Cl:1][C:2]1[CH:10]=[CH:9][C:8]([S:11](Cl)(=[O:13])=[O:12])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].[NH:15]1[CH2:20][CH2:19][CH:18]([CH2:21][OH:22])[CH2:17][CH2:16]1>C(Cl)Cl>[Cl:1][C:2]1[CH:10]=[CH:9][C:8]([S:11]([N:15]2[CH2:20][CH2:19][CH:18]([CH2:21][OH:22])[CH2:17][CH2:16]2)(=[O:13])=[O:12])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5]

参加物

4

反応物 2

HCID 67306Benzoic acid, 2-chloro-5-(chlorosulfonyl)-HCID 4207714-Piperidinemethanol

生成物 1

HCID 20505867HCID 20505867、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

2-Chloro-5-chlorosulfonylbenzoic acid (5.0 g.) is added to a solution of 4-piperidyl carbinol (6.9 g.) in 40 ml. of methylene chloride. The solution is refluxed for 2 hours, cooled to room temperature and stirred overnight. The solution is evaporated to dryness, the gummy residue dissolved in 1 N sodium hydroxide, and the alkaline solution extracted twice with ether. The aqueous solution is acidified with concentrated hydrochloric acid, and the precipitate recovered by filtration. Recrystallization from ethyl acetate yields crystals, m.p. 185°-187° C.

後処理

  1. temperatureThe solution is refluxed for 2 hours
  2. customThe solution is evaporated to dryness
  3. dissolutionthe gummy residue dissolved in 1 N sodium hydroxide
  4. extractionthe alkaline solution extracted twice with ether
  5. filtrationthe precipitate recovered by filtration
  6. customRecrystallization from ethyl acetate
  7. customyields crystals, m.p. 185°-187° C.

出典と根拠

ORDレコード
ord-37bfdf2cf16e4d66871ca50ca34985de
出典データセット
uspto-grants-1983_03
特許番号
US04377521

関連ノート

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