Dichloromethane methanol → 4-Cyclopropylpyridin-3-amine

HRID 705360노트

반응식

HRID 705360 반응식
[CH:1]1([C:4]2[CH:9]=[CH:8][N:7]=[CH:6][C:5]=2[NH:10]C(=O)OC(C)(C)C)[CH2:3][CH2:2]1.CO.C(Cl)Cl>Cl.O1CCOCC1>[CH:1]1([C:4]2[CH:9]=[CH:8][N:7]=[CH:6][C:5]=2[NH2:10])[CH2:3][CH2:2]1

참가 물질

5

반응물 2

HCID 21226129Dichloromethane methanolHCID 67981637Tert-butyl 4-cyclopropylpyridin-3-ylcarbamate

생성물 1

HCID 668019694-Cyclopropylpyridin-3-amine수율 144.4%

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매HCID 312751,4-Dioxane용매

실험 절차

Tert-butyl 4-cyclopropylpyridin-3-ylcarbamate (393 mg, 1.677 mmol) was dissolved in 4 M HCl in dioxane (30 mL), and stirred at room temperature for 1 hour, the reaction rapidly becoming a white heterogeneous mixture. TLC (SiO2, 5% methanol/CH2Cl2) showed reaction complete after 1 hour. The solvent was removed by rotary evaporation, the residue was triturated with diethyl ether and vacuum filtered to collect the solid, and the solid was dried in a vacuum oven at 50° C. for 1 hour to afford the product as a beige solid (325 mg).

후처리

  1. customthe reaction
  2. customreaction complete after 1 hour
  3. customThe solvent was removed by rotary evaporation
  4. customthe residue was triturated with diethyl ether and vacuum
  5. filtrationfiltered
  6. customto collect the solid
  7. customthe solid was dried in a vacuum oven at 50° C. for 1 hour

출처 및 근거

ORD 기록
ord-35f586d1acbf46cd81d8712eaa622790
출처 데이터셋
uspto-grants-2015_11
특허 번호
US09173887B2

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