Dichloromethane methanol → 4-Cyclopropylpyridin-3-amine

HRID 705360ノート

反応式

HRID 705360 の反応式
[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

参加物

5

反応物 2

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

生成物 1

HCID 668019694-Cyclopropylpyridin-3-amine収率 144.4%

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 312751,4-Dioxane溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-35f586d1acbf46cd81d8712eaa622790
出典データセット
uspto-grants-2015_11
特許番号
US09173887B2

反応ノート

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