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Hydrochloric Acid → alpha-(4-(N-methylcarbamyl)aminosulfonyl-2-n-propylphenoxy)-3,4-methylenedioxyphenylacetic acid

HRID 1378872
ノート
印刷プレビュー

反応式

HRID 1378872 の反応式
[CH3:1][NH:2][C:3]([NH:5][S:6]([C:9]1[CH:29]=[CH:28][C:12]([O:13][CH:14]([C:19]2[CH:24]=[CH:23][C:22]3[O:25][CH2:26][O:27][C:21]=3[CH:20]=2)[C:15]([O:17]C)=[O:16])=[C:11]([CH2:30][CH2:31][CH3:32])[CH:10]=1)(=[O:8])=[O:7])=[O:4].[OH-].[Na+].C(Cl)(Cl)Cl.CO.C(O)(=O)C.Cl>CO.O>[CH3:1][NH:2][C:3]([NH:5][S:6]([C:9]1[CH:29]=[CH:28][C:12]([O:13][CH:14]([C:19]2[CH:24]=[CH:23][C:22]3[O:25][CH2:26][O:27][C:21]=3[CH:20]=2)[C:15]([OH:17])=[O:16])=[C:11]([CH2:30][CH2:31][CH3:32])[CH:10]=1)(=[O:7])=[O:8])=[O:4]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 21866353chloroform methanol HOAcHCID 53963621methyl alpha-(4-(N-methylcarbamyl)aminosulfonyl-2-n-propylphenoxy)-3,4-methylenedioxyphenylacetate

生成物 1

HCID 53812605alpha-(4-(N-methylcarbamyl)aminosulfonyl-2-n-propylphenoxy)-3,4-methylenedioxyphenylacetic acid収率 70%

試薬・触媒・溶媒

2
HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

To a stirred solution of 570 mg (1.23 mmol) of the product of Step A in 6 mL of methanol was added 540 μL (2.71 mmol) of 5N sodium hydroxide. The reaction mixture was allowed to stir overnight after which TLC analysis (90:10:1 chloroform/methanol/acetic acid) indicated the saponification had proceeded to completion. The reaction mixture was acidified to pH=2 using 6N HCl, poured into water, and extracted with ethyl acetate. The extract was dried over magnesium sulfate, filtered and evaporated in vacuo to give the crude product. Purification of the crude product by silica-gel flash chromatography using (92:7:1 chloroform/methanol/acetic acid) afforded 384 mg (70%) of the title compound as an amorphous solid.

後処理

  1. extractionextracted with ethyl acetate
  2. dry with materialThe extract was dried over magnesium sulfate
  3. filtrationfiltered
  4. customevaporated in vacuo
  5. customto give the crude product
  6. customPurification of the crude product by silica-gel flash chromatography

出典と根拠

ORDレコード
ord-7133d350f535422a820905cc32a1e0d1
出典データセット
uspto-grants-1997_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05668176

反応ノート

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