Hydrochloric Acid → alpha-(4-Tert-butyldimethylsilyloxymethyl-2-n-propylphenoxy)-3,4-methylenedioxyphenylacetic acid

HRID 1378851ノート

反応式

HRID 1378851 の反応式
[Si:1]([O:8][CH2:9][C:10]1[CH:30]=[CH:29][C:13]([O:14][CH:15]([C:20]2[CH:25]=[CH:24][C:23]3[O:26][CH2:27][O:28][C:22]=3[CH:21]=2)[C:16]([O:18]C)=[O:17])=[C:12]([CH2:31][CH2:32][CH3:33])[CH:11]=1)([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2].[OH-].[Na+].C(Cl)(Cl)Cl.CO.[NH4+].[OH-].Cl>CO.ClCCl>[Si:1]([O:8][CH2:9][C:10]1[CH:30]=[CH:29][C:13]([O:14][CH:15]([C:20]2[CH:25]=[CH:24][C:23]3[O:26][CH2:27][O:28][C:22]=3[CH:21]=2)[C:16]([OH:18])=[O:17])=[C:12]([CH2:31][CH2:32][CH3:33])[CH:11]=1)([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 21873181Chloroform methanol ammonium hydroxideHCID 22912473Methyl alpha-(4-tert-butyldimethylsilyloxymethyl-2-n-propylphenoxy)-3,4-methylenedioxyphenylacetate

生成物 1

HCID 19080469alpha-(4-Tert-butyldimethylsilyloxymethyl-2-n-propylphenoxy)-3,4-methylenedioxyphenylacetic acid

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 6344Dichloromethane溶媒

実験手順

To a solution of 3.20 g (6.78 mmol) of the product of Step B dissolved in 10 mL of methanol and 3 mL of dichloromethane was added 1.42 mL (7.12 mmol) of a 5.0N aqueous solution of sodium hydroxide and the reaction mixture was magnetically stirred at room temperature. After 4 hours TLC analysis (CHCl3 --MeOH--NH4OH 80:15:1) indicated complete hydrolysis and the reaction mixture was adjusted to pH=4 with 1.0N HCl. The reaction mixture was then completely evaporated and dried in vacuo to afford the crude product which was used directly in the next step.

後処理

  1. customhydrolysis
  2. customThe reaction mixture was then completely evaporated
  3. customdried in vacuo

出典と根拠

ORDレコード
ord-04366f2f661b427990e5f73159c96d51
出典データセット
uspto-grants-1997_09
特許番号
US05668176

反応ノート

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