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Methanol → HCID 178426048, 화합물

HRID 1501120
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HRID 1501120 반응식
[F:1][C:2]([F:10])([F:9])[C:3](=O)[CH2:4][C:5](=O)[CH3:6].[C:11](#[N:15])[CH2:12][C:13]#[N:14].C[OH:17]>>[OH:17][C:11]1[N:15]=[C:5]([CH3:6])[CH:4]=[C:3]([C:2]([F:10])([F:9])[F:1])[C:12]=1[C:13]#[N:14]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 887MethanolHCID 8010MalononitrileHCID 739431,1,1-Trifluoro-2,4-pentanedione

생성물 1

HCID 178426048HCID 178426048, 화합물수율 40%

실험 절차

To a solution of 1,1,1-trifluoropentane-2,4-dione (5.8 g, 37.7 mmol) in methanol (20 mL) was added malononitrile (5 g, 75 mmol) and then the mixture was heated to reflux. The mixture was maintained at the same temperature for 12 hours. The resultant mixture was cooled to room temperature, and then filtered. The solid was washed with methanol to give pure 2-hydroxy-6-methyl-4-(trifluoromethyl)nicotinonitrile (3 g, 40%). 1H NMR (300 MHz, d6-DMSO): δ 13.36 (s, 1H), 6.65 (s, 1H), 2.38 (s, 3H).

후처리

  1. temperaturethe mixture was heated to reflux
  2. temperatureThe mixture was maintained at the same temperature for 12 hours
  3. filtrationfiltered
  4. washThe solid was washed with methanol

출처 및 근거

ORD 기록
ord-1fbe9f5604f8401488328216e84beba0
출처 데이터셋
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09206128B2

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