Hydrochloric Acid → 4-methoxy-2-(1H-pyrazol-1-yl)butanoic acid

HRID 887151ノート

反応式

HRID 887151 の反応式
[CH3:1][O:2][CH2:3][CH2:4][CH:5]([N:10]1[CH:14]=[CH:13][CH:12]=[N:11]1)[C:6]([O:8]C)=[O:7].[OH-].[K+].Cl>CO.O>[CH3:1][O:2][CH2:3][CH2:4][CH:5]([N:10]1[CH:14]=[CH:13][CH:12]=[N:11]1)[C:6]([OH:8])=[O:7]

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 14797Potassium HydroxideHCID 66839386Methyl 4-methoxy-2-(1H-pyrazol-1-yl)butanoate

生成物 1

HCID 579074424-methoxy-2-(1H-pyrazol-1-yl)butanoic acid収率 95%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

To a stirred solution of 0.045 g (0.23 mmol) of methyl 4-methoxy-2-(1H-pyrazol-1-yl)butanoate from step A above in 2 mL of methanol was added a solution of 0.032 g (0.57 mmol) of potassium hydroxide in 0.5 mL of water. The mixture was stirred at ambient temperature for 1.5 h then acidified with a 2 N hydrochloric acid solution until a pH of 4 was achieved. The mixture was evaporated to remove all volatiles then extracted with ethyl acetate. The combined extracts were washed with brine, dried over magnesium sulfate, filtered and evaporated to dryness to afford the title compound (0.040 g, 95%). LC-MS: m/z (ES) 185 (MH)+.

後処理

  1. customThe mixture was evaporated
  2. customto remove all volatiles
  3. extractionthen extracted with ethyl acetate
  4. washThe combined extracts were washed with brine
  5. dry with materialdried over magnesium sulfate
  6. filtrationfiltered
  7. customevaporated to dryness

出典と根拠

ORDレコード
ord-3b37b3f1af5f4f5c8f59a5f859028591
出典データセット
uspto-grants-2012_08
特許番号
US08247415B2

反応ノート

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