Hydrochloric Acid → [1-(tert-Butoxycarbonyl)piperidin-4-yl]acetic acid

HRID 1004506ノート

反応式

HRID 1004506 の反応式
C([O:3][C:4](=[O:19])[CH2:5][CH:6]1[CH2:11][CH2:10][N:9]([C:12]([O:14][C:15]([CH3:18])([CH3:17])[CH3:16])=[O:13])[CH2:8][CH2:7]1)C.[OH-].[Na+].Cl>CO.O>[C:15]([O:14][C:12]([N:9]1[CH2:10][CH2:11][CH:6]([CH2:5][C:4]([OH:19])=[O:3])[CH2:7][CH2:8]1)=[O:13])([CH3:18])([CH3:16])[CH3:17]

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 9993342Ethyl 1-((1,1-dimethylethoxy)carbonyl)-4-piperidineacetate

生成物 1

HCID 1512539[1-(tert-Butoxycarbonyl)piperidin-4-yl]acetic acid

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

The compound (5.28 g) obtained in the above (1) is dissolved in methanol (32 ml), and thereto is added 1N aqueous sodium hydroxide solution (23.4 ml), and the mixture is stirred at room temperature for three hours. The reaction mixture is diluted with water, and the pH value thereof is adjusted to pH 2 with 1N hydrochloric acid, and extracted three time with ethyl acetate. The extract is washed twice with a saturated brine, and dried over anhydrous magnesium sulfate. The desiccant is removed by filtration, and the filtrate is concentrated under reduced pressure to give the title compound (5.18 g).

後処理

  1. extractionextracted three time with ethyl acetate
  2. washThe extract is washed twice with a saturated brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customThe desiccant is removed by filtration
  5. concentrationthe filtrate is concentrated under reduced pressure

出典と根拠

ORDレコード
ord-df2746bd773e4f74aa6a4e47e5fc6a29
出典データセット
uspto-grants-2000_04
特許番号
US06048854

反応ノート

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