Propylamine → HCID 19960061, 화합물

HRID 2380221노트

반응식

HRID 2380221 반응식
Cl[C:2]1[C:7]([C:8]([NH:10][C:11]2[C:12]([Cl:17])=[N:13][CH:14]=[CH:15][CH:16]=2)=[O:9])=[CH:6][CH:5]=[CH:4][N:3]=1.[CH2:18]([NH2:21])[CH2:19][CH3:20]>O1CCOCC1>[Cl:17][C:12]1[C:11]([NH:10][C:8]([C:7]2[C:2]([NH:21][CH2:18][CH2:19][CH3:20])=[N:3][CH:4]=[CH:5][CH:6]=2)=[O:9])=[CH:16][CH:15]=[CH:14][N:13]=1

참가 물질

4

반응물 2

HCID 7852PropylamineHCID 27475382-chloro-N-(2-chloropyridin-3-yl)pyridine-3-carboxamide

생성물 1

HCID 19960061HCID 19960061, 화합물

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

반응 조건

온도
150 °C

실험 절차

26.8 g (0.1 mol) of 2-chloro-N-(2-chloro-3-pyridinyl)-3-pyridinecarboxamide were dissolved in 200 ml of dioxane, and the resulting solution was admixed with 21.4 g (0.362 mol) of propylamine. Thereafter, the mixture was shaken in a stainless steel pressure vessel at 150° C. for 6 hours. The reaction mixture was then evaporated in vacuo, and the residue was purified by column chromatography on silica gel, successively using dichloromethane/ethyl acetate 10/1 (v/v) and dichloromethane/cyclohexane/ethyl acetate 1/2/1 (v/v/v) as eluents. The product obtained by evaporation was a highly viscous resin that had a satisfactory quality for the following reaction.

후처리

  1. customThe reaction mixture was then evaporated in vacuo
  2. customthe residue was purified by column chromatography on silica gel, successively using dichloromethane/ethyl acetate 10/1 (v/v) and dichloromethane/cyclohexane/ethyl acetate 1/2/1 (v/v/v) as eluents
  3. customThe product obtained by evaporation
  4. customfor the following reaction

출처 및 근거

ORD 기록
ord-ca2ce2ce1ef440dba96579fa866d0b26
출처 데이터셋
uspto-grants-1994_11
특허 번호
US05366972

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