HCID 2728499, 화합물 → HCID 83486524, 화합물

HRID 1501123노트

반응식

HRID 1501123 반응식
[CH3:1][O:2][C:3]1[N:10]=[C:9]([CH3:11])[CH:8]=[C:7]([C:12]([F:15])([F:14])[F:13])[C:4]=1[C:5]#[N:6]>C(O)C.O.NN.[Ni]>[CH3:1][O:2][C:3]1[C:4]([CH2:5][NH2:6])=[C:7]([C:12]([F:15])([F:13])[F:14])[CH:8]=[C:9]([CH3:11])[N:10]=1

참가 물질

6

반응물 1

HCID 2728499HCID 2728499, 화합물

생성물 1

HCID 83486524HCID 83486524, 화합물수율 79.1%

시약·촉매·용매 4

HCID 935Nickel촉매HCID 702Ethanol용매HCID 962Water용매HCID 9321Hydrazine용매

반응 조건

온도
60 °C

실험 절차

To a solution of 2-methoxy-6-methyl-4-(trifluoromethyl)nicotinonitrile (0.6 g, 2.7 mmol) in ethanol (50 mL) was added the suspension of raney-Ni in water (1 mL) and hydrazine (5 mL). After stirring at 60° C. for 3 hours, the mixture was filtered and concentrated to give a residue. The residue was purified by chromatography (dichloromethane/methanol=10:1) to give (2-methoxy-6-methyl-4-(trifluoromethyl)pyridin-3-yl)methanamine (0.47 g, 77%) and used directly in next step without further purification. LRMS (M+H) m/z: calcd 220.08. found 220.

후처리

  1. filtrationthe mixture was filtered
  2. concentrationconcentrated
  3. customto give a residue
  4. customThe residue was purified by chromatography (dichloromethane/methanol=10:1)

출처 및 근거

ORD 기록
ord-9f6ab0cbdc564c54b7c4059f88b39a81
출처 데이터셋
uspto-grants-2015_12
특허 번호
US09206128B2

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