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Hydrochloric Acid → 2-Thiazolecarboxaldehyde, 5-(2,2,2-trifluoro-1-hydroxyethyl)-

HRID 1881886
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HRID 1881886 반응식
[O:1]1CCO[CH:2]1[C:6]1[S:7][C:8]([CH:11]([OH:16])[C:12]([F:15])([F:14])[F:13])=[CH:9][N:10]=1.Cl.O1CCCC1>O>[F:14][C:12]([F:13])([F:15])[CH:11]([C:8]1[S:7][C:6]([CH:2]=[O:1])=[N:10][CH:9]=1)[OH:16]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 8028TetrahydrofuranHCID 593313011-[2-(1,3-Dioxolan-2-yl)-1,3-thiazol-5-yl]-2,2,2-trifluoroethanol

생성물 1

HCID 593313142-Thiazolecarboxaldehyde, 5-(2,2,2-trifluoro-1-hydroxyethyl)-수율 80%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of 1-[2-(1,3-dioxolan-2-yl)-1,3-thiazol-5-yl]-2,2,2-trifluoroethanol (2.56 g), 1M hydrochloric acid (10 mL) and tetrahydrofuran (10 mL) was stirred with heating under reflux for 6 hr. Water was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The ethyl acetate layer was washed with saturated brine, dried (MgSO4) and concentrated. The obtained residue was subjected to silica gel column chromatography, and the title compound (1.69 g, yield 80%) was obtained as colorless crystals from a fraction eluted with ethyl acetate-hexane (4:1, volume ratio). melting point 64-66° C.

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후처리

  1. temperaturewith heating
  2. temperatureunder reflux for 6 hr
  3. extractionthe mixture was extracted with ethyl acetate
  4. washThe ethyl acetate layer was washed with saturated brine
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-86427174221c443b97314867fd375ab7
출처 데이터셋
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08318746B2

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