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

HRID 846245
ノート
印刷プレビュー

反応式

HRID 846245 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 6569Methyl Ethyl Ketone
溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-16814c7e21d94d219db243fcf1e78f37
出典データセット
uspto-grants-1992_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05135940

反応ノート

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