Hydrochloric Acid → 2-[2-(4-Benzylamino-3-hydroxy-phenyl)-1-methyl-2-oxo-ethyl]-malonic acid

HRID 1619964ノート

反応式

HRID 1619964 の反応式
[CH2:1]([N:8]1[C:12]2[CH:13]=[CH:14][C:15]([C:17](=[O:31])[CH:18]([CH:20]([C:26]([O:28]CC)=[O:27])[C:21]([O:23]CC)=[O:22])[CH3:19])=[CH:16][C:11]=2[O:10]C1=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[OH-].[Na+].Cl>C(O)C>[CH2:1]([NH:8][C:12]1[CH:13]=[CH:14][C:15]([C:17](=[O:31])[CH:18]([CH:20]([C:26]([OH:28])=[O:27])[C:21]([OH:23])=[O:22])[CH3:19])=[CH:16][C:11]=1[OH:10])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium Hydroxide2 回HCID 67466180Diethyl 2-[2-(3-benzyl-2-oxo-2,3-dihydro-benzoxazol-6-yl)-1-methyl-2-oxo-ethyl]-malonate

生成物 1

HCID 674670302-[2-(4-Benzylamino-3-hydroxy-phenyl)-1-methyl-2-oxo-ethyl]-malonic acid

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

5 g (11.4 mmol) diethyl 2-[2-(3-benzyl-2-oxo-2,3-dihydro-benzoxazol-6-yl)-1-methyl-2-oxo-ethyl]-malonate are combined with 50 ml of ethanol, then 28 ml 1N sodium hydroxide solution are added and the mixture is stirred overnight at RT. The next day another 28 ml of 1N sodium hydroxide solution are added and the mixture is refluxed for 6 h. After cooling to RT 50 ml 1N hydrochloric acid are added and the mixture is extracted with DCM. The phases are separated using a phase transfer cartridge. The filtrate is evaporated down i. V.

後処理

  1. temperaturethe mixture is refluxed for 6 h
  2. additionare added
  3. extractionthe mixture is extracted with DCM
  4. customThe phases are separated
  5. customThe filtrate is evaporated down i

出典と根拠

ORDレコード
ord-2acfb75b7cfa407fa6d966a68c38ed75
出典データセット
uspto-grants-2014_07
特許番号
US08772323B2

反応ノート

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