Water → 4-((2,2-Dimethyl-1,3-dioxolan-4-yl)methoxy)pyridin-2-amine

HRID 79436

반응식

HRID 79436 반응식
Cl[C:2]1[CH:7]=[CH:6][N:5]=[C:4]([NH2:8])[CH:3]=1.[CH3:9][C:10]1([CH3:17])[O:14][CH:13]([CH2:15][OH:16])[CH2:12][O:11]1.[Na].O>ClCCl>[CH3:9][C:10]1([CH3:17])[O:14][CH:13]([CH2:15][O:16][C:2]2[CH:7]=[CH:6][N:5]=[C:4]([NH2:8])[CH:3]=2)[CH2:12][O:11]1

참가 물질

6

반응물 4

HCID 962WaterHCID 7528SolketalHCID 5818662-Amino-4-chloropyridineHCID 5360545Sodium

생성물 1

HCID 509875954-((2,2-Dimethyl-1,3-dioxolan-4-yl)methoxy)pyridin-2-amine수율 80%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
145 °C

실험 절차

A sealed tube containing 4-chloro-2-pyridinamine (4 g, 31.2 mmol), (2,2-dimethyl-1,3-dioxolan-4-yl)methanol (8.4 g, 60.6 mmol), and sodium (1.46 g, 63.5 mmol) was heated at 145° C. for 8 hours. The mixture was cooled to ambient temperature; water (25 mL) and dichloromethane (50 mL) were added. The organic phase was separated, dried with sodium sulfate, and concentrated under reduced pressure. The resulting residue was purified by chromatography on silica-gel to give 4-((2,2-dimethyl-1,3-dioxolan-4-yl)methoxy)pyridin-2-amine as a pale yellow solid (5.6 g).

후처리

  1. temperatureThe mixture was cooled to ambient temperature
  2. customThe organic phase was separated
  3. dry with materialdried with sodium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe resulting residue was purified by chromatography on silica-gel

출처 및 근거

ORD 기록
ord-5231720e43f441fda1d0c65964eaca65
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08841455B2

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