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2-(1-Methylhydrazinyl)-3-(trifluoromethyl)pyridine → HCID 53949563, 화합물

HRID 1106708
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인쇄 미리보기

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HRID 1106708 반응식
[Cl:1][C:2]1[N:6]([C:7]2[CH:14]=[CH:13][CH:12]=[CH:11][C:8]=2[CH:9]=O)[C:5](=[O:15])[N:4]([CH3:16])[N:3]=1.[F:17][C:18]([F:29])([F:28])[C:19]1[C:20]([N:25]([CH3:27])[NH2:26])=[N:21][CH:22]=[CH:23][CH:24]=1>C(O)C.C(O)(=O)C.C(=O)(O)[O-].[Na+]>[Cl:1][C:2]1[N:6]([C:7]2[CH:14]=[CH:13][CH:12]=[CH:11][C:8]=2[CH:9]=[N:26][N:25]([CH3:27])[C:20]2[C:19]([C:18]([F:29])([F:28])[F:17])=[CH:24][CH:23]=[CH:22][N:21]=2)[C:5](=[O:15])[N:4]([CH3:16])[N:3]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 2

HCID 27777792-(1-Methylhydrazinyl)-3-(trifluoromethyl)pyridineHCID 18789809HCID 18789809, 화합물

생성물 1

HCID 53949563HCID 53949563, 화합물

시약·촉매·용매 3

HCID 176Acetic Acid촉매HCID 702Ethanol용매2회HCID 516892Sodium Bicarbonate용매

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온도
50 °C

실험 절차

The title compound of Step A (0.20 g, 0.80 mmol) was dissolved in absolute ethanol (7 mL) and a solution of 1-[3-(trifluoromethyl)pyridin-2-yl]-1-methylhydrazine in ethanol (3 mL) was added followed by 3 drops of glacial acetic acid. The mixture was warmed to 50° C. for 1 h, cooled to room temperature and then diluted with aqueous sodium bicarbonate and extracted three times with ethyl acetate. The combined organic phases were dried (MgSO4), filtered and concentrated to give 0.38 g of the title compound of Step B as a yellow solid. 1H NMR (300 MHz. CDCl3): δ 8.42 (d.1H. J=5 Hz), 8.16 (d,1H, J=8 Hz), 8.01 (d,1H, J=8 Hz), 7.51 (t,1H, J=8 Hz), 7.42 (t,1H), J=8 Hz), 7.35 (s,1H), 7.21 (d,1H, J=8 Hz), 7.03 (dd,1H, J=8, 5 Hz), 3.56 (s,6H).

후처리

  1. temperaturecooled to room temperature
  2. extractionextracted three times with ethyl acetate
  3. dry with materialThe combined organic phases were dried (MgSO4)
  4. filtrationfiltered
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-0a5a06c4bc3c411dbd7bff557fa6592a
출처 데이터셋
uspto-grants-2000_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06057352

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