HCID 57736454, 화합물 → 6-(Difluoromethyl)pyridin-3-amine

HRID 1641765노트

반응식

HRID 1641765 반응식
C(OC(=O)[NH:7][C:8]1[CH:9]=[N:10][C:11]([CH:14]([F:16])[F:15])=[CH:12][CH:13]=1)(C)(C)C>ClCCl.FC(F)(F)C(O)=O>[F:15][CH:14]([F:16])[C:11]1[N:10]=[CH:9][C:8]([NH2:7])=[CH:13][CH:12]=1

참가 물질

4

반응물 1

HCID 57736454HCID 57736454, 화합물

생성물 1

HCID 552816746-(Difluoromethyl)pyridin-3-amine수율 82.6%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 6422Trifluoroacetic acid용매

실험 절차

To a solution of tert-butyl[6-(difluoromethyl)pyridin-3-yl]carbamate (1.11 g, 4.54 mmol) in dichloromethane (8 ml), trifluoroacetic acid (8 ml) was added at room temperature. The reaction mixture was stirred for 5 hours at the same temperature, and then was concentrated under reduced pressure. Dichloromethane and saturated aqueous sodium hydrogencarbonate were added to the resulting residue. The organic layer was taken, and the organic layer was dried over anhydrous sodium sulfate and filtered. Subsequently, the filtrate was concentrated under reduced pressure. The resulting residue was subjected to flash silica gel chromatography, and the fraction obtained from an elution with hexane:ethyl acetate=2:1 was concentrated under reduced pressure to obtain the title compound (540 mg, 3.75 mmol, 82%) as a pale green oily substance.

후처리

  1. concentrationwas concentrated under reduced pressure
  2. additionDichloromethane and saturated aqueous sodium hydrogencarbonate were added to the resulting residue
  3. dry with materialthe organic layer was dried over anhydrous sodium sulfate
  4. filtrationfiltered
  5. concentrationSubsequently, the filtrate was concentrated under reduced pressure
  6. customthe fraction obtained from an elution with hexane
  7. concentrationethyl acetate=2:1 was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-34fdfdc303ef4dff9a9624d71868562e
출처 데이터셋
uspto-grants-2012_02
특허 번호
US08114886B2

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