Hydrochloric Acid → 2-Tert-butoxycarbonylamino-3-(2-hydroxy-4-methoxy-phenyl)propanoic acid

HRID 540413ノート

反応式

HRID 540413 の反応式
[OH-].[Na+].[C:3]([O:7][C:8]([NH:10][CH:11]([CH2:16][C:17]1[CH:22]=[CH:21][C:20]([O:23][CH3:24])=[CH:19][C:18]=1[OH:25])[C:12]([O:14]C)=[O:13])=[O:9])([CH3:6])([CH3:5])[CH3:4].Cl>O1CCCC1>[C:3]([O:7][C:8]([NH:10][CH:11]([CH2:16][C:17]1[CH:22]=[CH:21][C:20]([O:23][CH3:24])=[CH:19][C:18]=1[OH:25])[C:12]([OH:14])=[O:13])=[O:9])([CH3:5])([CH3:6])[CH3:4]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 397418Methyl 2-tert-butoxycarbonylamino-3-(2-hydroxy-4-methoxyphenyl)-propanoate

生成物 1

HCID 669881482-Tert-butoxycarbonylamino-3-(2-hydroxy-4-methoxy-phenyl)propanoic acid収率 101.3%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

5 ml of a 1N aqueous solution of sodium hydroxide are added to a solution of 850 mg (2.6 mmol) of methyl 2-tert-butoxycarbonylamino-3-(2-hydroxy-4-methoxyphenyl)-propanoate in 10 ml of tetrahydrofuran. The reaction medium is stirred for 4 hours at ambient temperature and then a 1N aqueous solution of hydrochloric acid is added until the pH is 1, and the medium is extracted with dichloromethane. The organic phase is dried over magnesium sulphate, filtered and evaporated. 820 mg of 2-tert-butoxycarbonylamino-3-(2-hydroxy-4-methoxy-phenyl)propanoic acid are obtained in the form of a beige powder with a quantitative yield.

後処理

  1. extractionthe medium is extracted with dichloromethane
  2. dry with materialThe organic phase is dried over magnesium sulphate
  3. filtrationfiltered
  4. customevaporated

出典と根拠

ORDレコード
ord-807e9f4bda234db3b1d8b8f9f36c4a67
出典データセット
uspto-grants-2014_10
特許番号
US08871187B2

反応ノート

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