Hydrochloric Acid → 2-(2-Methylpropyl)-1,3-thiazole-4-carboxylic acid

HRID 471155

反応式

HRID 471155 の反応式
O.[OH-].[Li+].[CH2:4]([C:8]1[S:9][CH:10]=[C:11]([C:13]([O:15]CC)=[O:14])[N:12]=1)[CH:5]([CH3:7])[CH3:6].Cl>C1COCC1.O>[CH2:4]([C:8]1[S:9][CH:10]=[C:11]([C:13]([OH:15])=[O:14])[N:12]=1)[CH:5]([CH3:7])[CH3:6]

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 168937Lithium hydroxide, monohydrateHCID 11608194Ethyl 2-isobutylthiazole-4-carboxylate

生成物 1

HCID 235881542-(2-Methylpropyl)-1,3-thiazole-4-carboxylic acid

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

Lithium hydroxide monohydrate (4.1 g) was added to a solution of ethyl 2-isobutylthiazole-4-carboxylate (example 72, step c) (5.2 g) in a mixture of THF (80 mL) and water (20 mL). The resulting mixture was stirred overnight. The reaction was carefully acidified with concentrated hydrochloric acid (10 mL) and the volatiles evaporated. The resulting aqueous mixture was poured into brine (50 mL) and extracted with ethyl acetate (3×100 mL). The combined organic solutions were washed with brine (50 mL), dried over sodium sulphate, filtered and evaporated to give the subtitled compound as a white solid. Yield 3.8 g.

後処理

  1. customthe volatiles evaporated
  2. additionThe resulting aqueous mixture was poured into brine (50 mL)
  3. extractionextracted with ethyl acetate (3×100 mL)
  4. washThe combined organic solutions were washed with brine (50 mL)
  5. dry with materialdried over sodium sulphate
  6. filtrationfiltered
  7. customevaporated

出典と根拠

ORDレコード
ord-111055d98e144a6eaf02c32065a8ba5b
出典データセット
uspto-grants-2014_01
特許番号
US08629271B2

関連ノート

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