Ethanol → HCID 54230349, 화합물

HRID 1085955노트

반응식

HRID 1085955 반응식
[N:1]1[CH:6]=[CH:5][C:4]([C:7]([CH2:9][CH2:10][CH2:11][CH3:12])=O)=[CH:3][CH:2]=1.[C:13]([O:17][CH2:18][CH3:19])(=[O:16])[NH:14][NH2:15].C(O)C>C1(C)C=CC(S(O)(=O)=O)=CC=1.CO.C(Cl)Cl>[N:1]1[CH:6]=[CH:5][C:4]([C:7](=[N:15][NH:14][C:13]([O:17][CH2:18][CH3:19])=[O:16])[CH2:9][CH2:10][CH2:11][CH3:12])=[CH:3][CH:2]=1

참가 물질

6

반응물 3

HCID 702EthanolHCID 20064Hydrazinecarboxylic acid, ethyl esterHCID 743441-Pentanone, 1-(4-pyridyl)-

생성물 1

HCID 54230349HCID 54230349, 화합물수율 54%

시약·촉매·용매 2

HCID 6101p-Toluenesulfonic acid촉매HCID 21226129Dichloromethane methanol용매

실험 절차

A mixture of 8.3 gm (0.055 mole) of n-butyl 4-pyridyl ketone, 6.1 gm (0.059 mole) of ethyl carbazate and 150 ml of absolute ethanol is refluxed 17 hr. A Tlc (3% MeOH/CH2Cl2 on Silica gel) shows 50% starting material remaining. p-Toluenesulfonic acid (0.3 gm) is added and the reaction mixture refluxed 17 hr more. Tlc shows no remaining starting materials. The reaction is concentrated in vacuo. The residue is slurried with water and the solid collected, washed with water and dried. Crystallization yields 7.41 gm of the title compound having a melting point of 102.1° C.

후처리

  1. temperatureis refluxed 17 hr
  2. temperaturethe reaction mixture refluxed 17 hr more
  3. concentrationThe reaction is concentrated in vacuo
  4. customthe solid collected
  5. washwashed with water
  6. customdried
  7. customCrystallization

출처 및 근거

ORD 기록
ord-b80ab66bd86d4683a0b09c6ac972c5de
출처 데이터셋
uspto-grants-1991_04
특허 번호
US05011932

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