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2-Aminothiazole → 2-(2-AMINO-1,3-THIAZOL-5-YL)-1,1,1,3,3,3-HEXAFLUOROPROPAN-2-OL

HRID 1807806
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HRID 1807806 반응식
[S:1]1[CH:5]=[CH:4][N:3]=[C:2]1[NH2:6].O.O.O.[F:10][C:11]([F:19])([F:18])[C:12]([C:14]([F:17])([F:16])[F:15])=[O:13]>C(OCC)(=O)C>[NH2:6][C:2]1[S:1][C:5]([C:12]([OH:13])([C:14]([F:17])([F:16])[F:15])[C:11]([F:19])([F:18])[F:10])=[CH:4][N:3]=1
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참가 물질

4

반응물 2

HCID 21552-AminothiazoleHCID 36719Hexafluoroacetone trihydrate

생성물 1

HCID 23180662-(2-AMINO-1,3-THIAZOL-5-YL)-1,1,1,3,3,3-HEXAFLUOROPROPAN-2-OL수율 32.3%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

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온도
100 °C

실험 절차

Thiazol-2-amine (150 mmol, 15 g), 4 Å powdered molecular sieves (1 g) and hexafluoroacetone trihydrate (300 mmol, 65.9 g) were combined and heated to 100° C. for 16 hours. The reaction mixture was cooled, diluted with ethyl acetate (200 mL) and filtered through celite. The filtrate was concentrated under reduced pressure to give a brown liquid which crystallised on standing. The solid was collected by filtration, washed with heptane (100 mL) then diethyl ether (50 mL) and dried under vacuum to afford the title compound (12.9 g). MS (ESI) m/z 266.7 [M+H]+

후처리

  1. temperatureThe reaction mixture was cooled
  2. filtrationfiltered through celite
  3. concentrationThe filtrate was concentrated under reduced pressure
  4. customto give a brown liquid which
  5. customcrystallised
  6. filtrationThe solid was collected by filtration
  7. washwashed with heptane (100 mL)
  8. dry with materialdiethyl ether (50 mL) and dried under vacuum

출처 및 근거

ORD 기록
ord-9b2a59b4a77f43ec80ebbf9ed24793b7
출처 데이터셋
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08357679B2

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