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Potassium Carbonate → Methyl 4-(3-(4-acetyl-3-hydroxy-2-propylphenoxy)propylthio)-gamma-oxo-beta-methyl-2-bromobenzenebutanoate

HRID 846245
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인쇄 미리보기

반응식

HRID 846245 반응식
[Br:1][C:2]1[CH:7]=[C:6]([SH:8])[CH:5]=[CH:4][C:3]=1[C:9](=[O:17])[CH:10]([CH3:16])[CH2:11][C:12]([O:14][CH3:15])=[O:13].[C:18]([C:21]1[CH:31]=[CH:30][C:24]([O:25][CH2:26][CH2:27][CH2:28]Br)=[C:23]([CH2:32][CH2:33][CH3:34])[C:22]=1[OH:35])(=[O:20])[CH3:19].C(=O)([O-])[O-].[K+].[K+]>C(C(C)=O)C.C(OCC)(=O)C>[C:18]([C:21]1[CH:31]=[CH:30][C:24]([O:25][CH2:26][CH2:27][CH2:28][S:8][C:6]2[CH:5]=[CH:4][C:3]([C:9](=[O:17])[CH:10]([CH3:16])[CH2:11][C:12]([O:14][CH3:15])=[O:13])=[C:2]([Br:1])[CH:7]=2)=[C:23]([CH2:32][CH2:33][CH3:34])[C:22]=1[OH:35])(=[O:20])[CH3:19]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 11430Potassium CarbonateHCID 27752211-[4-(3-Bromopropoxy)-2-hydroxy-3-propylphenyl]ethanoneHCID 19884853Methyl 2-bromo-4-mercapto-gamma-oxo-beta-methylbenzenebutanoate

생성물 1

HCID 19884798Methyl 4-(3-(4-acetyl-3-hydroxy-2-propylphenoxy)propylthio)-gamma-oxo-beta-methyl-2-bromobenzenebutanoate

시약·촉매·용매 2

HCID 6569Methyl Ethyl Ketone
용매
HCID 8857Ethyl Acetate용매

실험 절차

To a solution of the thiol from step C (2.9 g) and 3-(4-acetyl-3-hydroxy-2-propylphenoxy)propylbromide (3.74 g) in methyl ethyl ketone (25 c.c.) was added potassium carbonate (3.78 g, milled) and the suspension was refluxed for 21/2 hours, then stirred at R.T. for 12 hours. The mixture was diluted with ethyl acetate (25 c.c.) and the insolubles filtered off. The filtrate was concentrated to dryness in vacuo and the residue purified on silica gel to yield the title compound as an oil.

후처리

  1. temperaturethe suspension was refluxed for 21/2 hours
  2. filtrationthe insolubles filtered off
  3. concentrationThe filtrate was concentrated to dryness in vacuo
  4. customthe residue purified on silica gel

출처 및 근거

ORD 기록
ord-16814c7e21d94d219db243fcf1e78f37
출처 데이터셋
uspto-grants-1992_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05135940

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