HCID 57736454、化合物 → 6-(Difluoromethyl)pyridin-3-amine

HRID 1641765ノート

反応式

HRID 1641765 の反応式
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

参加物

4

反応物 1

HCID 57736454HCID 57736454、化合物

生成物 1

HCID 552816746-(Difluoromethyl)pyridin-3-amine収率 82.6%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 6422Trifluoroacetic acid溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-34fdfdc303ef4dff9a9624d71868562e
出典データセット
uspto-grants-2012_02
特許番号
US08114886B2

反応ノート

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