Water → 3-Isothiocyanato-6-methoxy-2-(trifluoromethyl)pyridine

HRID 1398953노트

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HRID 1398953 반응식
[CH3:1][O:2][C:3]1[N:8]=[C:7]([C:9]([F:12])([F:11])[F:10])[C:6]([NH2:13])=[CH:5][CH:4]=1.[C:14](Cl)(Cl)=[S:15].O>O1CCCC1.C(=O)([O-])O.[Na+]>[N:13]([C:6]1[C:7]([C:9]([F:10])([F:11])[F:12])=[N:8][C:3]([O:2][CH3:1])=[CH:4][CH:5]=1)=[C:14]=[S:15]

참가 물질

6

반응물 3

HCID 962WaterHCID 10040ThiophosgeneHCID 447547986-Methoxy-2-(trifluoromethyl)pyridin-3-amine

생성물 1

HCID 866329283-Isothiocyanato-6-methoxy-2-(trifluoromethyl)pyridine수율 99.7%

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 516892Sodium Bicarbonate용매

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온도
0 °C

실험 절차

To a solution of 6-methoxy-2-(trifluoromethyl)pyridin-3-amine (6.99 g, 36.4 mmol) in tetrahydrofuran (60 mL) and saturated aqueous sodium hydrogen carbonate (60 mL) was added dropwise thiophosgene (2.8 mL, 36.5 mmol) at 0° C. The mixture was stirred at 0° C. for 0.5 hr. Water was added to the reaction mixture and the mixture was extracted with ethyl acetate. The organic layer was washed with brine, dried over anhydrous magnesium sulfate, and concentrated in vacuo to give the title compound (8.49 g, 36.3 mmol, quant.) as a pale orange oil.

후처리

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe organic layer was washed with brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-7aafcb3b2fbf4e5485a33c5241236e39
출처 데이터셋
uspto-grants-2014_12
특허 번호
US08901141B2

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