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

HRID 1881886
ノート
印刷プレビュー

反応式

HRID 1881886 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  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

出典と根拠

ORDレコード
ord-86427174221c443b97314867fd375ab7
出典データセット
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08318746B2

反応ノート

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