Benzoic Acid → HCID 53707664, 화합물

HRID 427280노트

반응식

HRID 427280 반응식
[CH2:1]([O:3][CH:4]([O:15][CH2:16][CH3:17])[CH2:5][O:6][C:7]1[CH:14]=[CH:13][C:10]([CH:11]=O)=[CH:9][CH:8]=1)[CH3:2].[S:18]1[CH2:22][C:21](=[O:23])[NH:20][C:19]1=[O:24].C(O)(=O)C1C=CC=CC=1.N1CCCCC1>C1(C)C=CC=CC=1.CCOC(C)=O.O>[CH2:1]([O:3][CH:4]([O:15][CH2:16][CH3:17])[CH2:5][O:6][C:7]1[CH:14]=[CH:13][C:10]([CH:11]=[C:22]2[S:18][C:19](=[O:24])[NH:20][C:21]2=[O:23])=[CH:9][CH:8]=1)[CH3:2]

참가 물질

8

반응물 4

HCID 243Benzoic AcidHCID 5437ThiazolidinedioneHCID 8082PiperidineHCID 187608894-(2,2-Diethoxyethoxy)benzaldehyde

생성물 1

HCID 53707664HCID 53707664, 화합물수율 83.5%

시약·촉매·용매 3

HCID 962Water용매HCID 1140Toluene용매HCID 8857Ethyl Acetate용매

실험 절차

A mixture of 4-[(2,2-diethoxy]ethoxy]benzaldehyde (10.6 g, 44.53 mmol), thiazolidin-2,4-dione (5.21 g, 44.53 mmol), benzoic acid (0.70 g, 5.78 mmol) and piperidine (0.64 mL, 6.7 mmol) in toluene (150 mL) was refluxed for 2 h with continuous removal of water. The reaction mixture was cooled to room temperature and diluted with EtOAc (150 ml). The mixture was washed with water, brine, dried over anhydrous Na2SO4 and concentrated. The crude compound was purified by column chromatography using EtOAc:pet. ether (1:2) as eluent to afford the title compound (12.54 g, 70%) as a brown coloured liquid.

후처리

  1. washThe mixture was washed with water, brine
  2. dry with materialdried over anhydrous Na2SO4
  3. concentrationconcentrated
  4. customThe crude compound was purified by column chromatography

출처 및 근거

ORD 기록
ord-08dba9a98b3e4661a8399b6bf0ae5527
출처 데이터셋
uspto-grants-2001_11
특허 번호
US06313113B1

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