Sodium Hydroxide → 1-(2-Chloro-benzenesulfonyl)-4-(2-methoxy-ethyl)-piperidine-4-carboxylic acid

HRID 2194115노트

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HRID 2194115 반응식
C([O:3][C:4]([C:6]1([CH2:22][CH2:23][O:24][CH3:25])[CH2:11][CH2:10][N:9]([S:12]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=2[Cl:21])(=[O:14])=[O:13])[CH2:8][CH2:7]1)=[O:5])C.[OH-].[Na+]>CO>[Cl:21][C:16]1[CH:17]=[CH:18][CH:19]=[CH:20][C:15]=1[S:12]([N:9]1[CH2:8][CH2:7][C:6]([CH2:22][CH2:23][O:24][CH3:25])([C:4]([OH:5])=[O:3])[CH2:11][CH2:10]1)(=[O:13])=[O:14]

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 667876761-(2-Chloro-benzenesulfonyl)-4-(2-methoxy-ethyl)-piperidine-4-carboxylic acid ethyl ester

생성물 1

HCID 595780921-(2-Chloro-benzenesulfonyl)-4-(2-methoxy-ethyl)-piperidine-4-carboxylic acid수율 111.8%

시약·촉매·용매 1

HCID 887Methanol용매

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온도
60 °C

실험 절차

1-(2-Chloro-benzenesulfonyl)-4-(2-methoxy-ethyl)-piperidine-4-carboxylic acid ethyl ester (0.5 g) was dissolved in MeOH (8 ml), 3M aqueous NaOH (6.41 ml) was added and the mixture was stirred at 5 h at 60° C. to complete the reaction. The solvent was evaporated off, the residue was acidified with 3M aqueous HCl and extracted with dichloromethane. The layers were separated, the organic phase was washed with brine, dried over sodium sulphate and concentrated to give the desired 1-(2-chloro-benzenesulfonyl)-4-(2-methoxy-ethyl)-piperidine-4-carboxylic acid (0.519 g) as a light brown solid. MS (ESI): 360.1 (M-H)−.

후처리

  1. customthe reaction
  2. customThe solvent was evaporated off
  3. extractionextracted with dichloromethane
  4. customThe layers were separated
  5. washthe organic phase was washed with brine
  6. dry with materialdried over sodium sulphate
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-800c4c723c64418589bb6bd6c63a7c4a
출처 데이터셋
uspto-grants-2012_12
특허 번호
US08329904B2

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