Hydrochloric Acid → 2-Butyl-4-thiazolecarboxylic acid

HRID 1689405

반응식

HRID 1689405 반응식
[OH-].[Li+].[CH2:3]([C:7]1[S:8][CH:9]=[C:10]([C:12]([O:14]CC)=[O:13])[N:11]=1)[CH2:4][CH2:5][CH3:6].Cl>C1COCC1.O>[CH2:3]([C:7]1[S:8][CH:9]=[C:10]([C:12]([OH:14])=[O:13])[N:11]=1)[CH2:4][CH2:5][CH3:6]

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 3939Lithium HydroxideHCID 67292599Ethyl 2-butyl-1,3-thiazole-4-carboxylate

생성물 1

HCID 140500762-Butyl-4-thiazolecarboxylic acid

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

Lithium hydroxide (5.00 g) was added to a stirred mixture of ethyl 2-butylthiazole-4-carboxylate (example 78, step f) (6.50 g) in THF (80 mL) and water (20 mL). After 16 h, concentrated hydrochloric acid (10 mL) was added and the solution concentrated to ˜40 mL. The reaction mixture was partitioned between ethyl acetate and brine. The aqueous layer was extracted three times with ethyl acetate. The combined organic layers were dried over magnesium sulphate, filtered and evaporated in vacuo to give the subtitled compound as an off white solid. Yield 4.6 g.

후처리

  1. concentrationthe solution concentrated to ˜40 mL
  2. customThe reaction mixture was partitioned between ethyl acetate and brine
  3. extractionThe aqueous layer was extracted three times with ethyl acetate
  4. dry with materialThe combined organic layers were dried over magnesium sulphate
  5. filtrationfiltered
  6. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-1f35ce651f9a434492c6668fd1d79721
출처 데이터셋
uspto-grants-2012_04
특허 번호
US08148373B2

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