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

HRID 471155

반응식

HRID 471155 반응식
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]

참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-111055d98e144a6eaf02c32065a8ba5b
출처 데이터셋
uspto-grants-2014_01
특허 번호
US08629271B2

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