Sodium Hydroxide → HCID 13338867, 화합물

HRID 1285396노트

반응식

HRID 1285396 반응식
[C:1]([C:4]1[CH:26]=[CH:25][C:7]([O:8][CH2:9][CH2:10][CH2:11][O:12][C:13]2[CH:23]=[CH:22][C:16]([C:17]([O:19]CC)=[O:18])=[CH:15][C:14]=2[Br:24])=[C:6]([CH2:27][CH2:28][CH3:29])[C:5]=1[OH:30])(=[O:3])[CH3:2].[OH-].[Na+]>C(O)C>[C:1]([C:4]1[CH:26]=[CH:25][C:7]([O:8][CH2:9][CH2:10][CH2:11][O:12][C:13]2[CH:23]=[CH:22][C:16]([C:17]([OH:19])=[O:18])=[CH:15][C:14]=2[Br:24])=[C:6]([CH2:27][CH2:28][CH3:29])[C:5]=1[OH:30])(=[O:3])[CH3:2]

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 13338863Ethyl 4-[3-(4-acetyl-3-hydroxy-2-n-propylphenoxy)propoxy]-3-bromobenzoate

생성물 1

HCID 13338867HCID 13338867, 화합물수율 75.1%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of ethyl 4-[3-(4-acetyl-3-hydroxy-2-n-propylphenoxy)propoxy]-3-bromobenzoate (1.50 g), ethanol (15 ml) and 1N sodium hydroxide (10 ml) was refluxed for 0.5 hour, then concentrated, acidified with concentrated hydrochloric acid, and extracted with ethyl acetate. The extract was washed with water and dried over sodium sulfate, the solvent was distilled off, and the residue was chromatographed on a column of silica gel (50 g), and eluted with a solution of chloroform-acetone-formic acid (9:1:0.1). Recrystallization from ethyl acetate gave 4-[3-(4-acetyl-3-hydroxy-2-n-propylphenoxy)propoxy]-3-bromobenzoic acid as colorless needles (1.06 g). Melting point 180°-182° C.

후처리

  1. temperaturewas refluxed for 0.5 hour
  2. concentrationconcentrated
  3. extractionextracted with ethyl acetate
  4. washThe extract was washed with water
  5. dry with materialdried over sodium sulfate
  6. distillationthe solvent was distilled off
  7. customthe residue was chromatographed on a column of silica gel (50 g)
  8. washeluted with a solution of chloroform-acetone-formic acid (9:1:0.1)
  9. customRecrystallization from ethyl acetate

출처 및 근거

ORD 기록
ord-75f04f5dcca04340a853302afe1f1996
출처 데이터셋
uspto-grants-1986_01
특허 번호
US04567201

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