3-Amino-4-chlorophenol → HCID 136335905, 화합물

HRID 2266482노트

반응식

HRID 2266482 반응식
[NH2:1][C:2]1[CH:3]=[C:4]([OH:9])[CH:5]=[CH:6][C:7]=1[Cl:8].[CH3:10][S:11]([C:14]1[CH:27]=[CH:26][C:17]([CH2:18][CH:19]([C:23](=O)[CH3:24])[C:20](=O)[CH3:21])=[CH:16][CH:15]=1)(=[O:13])=[O:12]>CS(O)(=O)=O.C1(C)C=CC=CC=1>[Cl:8][C:7]1[C:2]2[N:1]=[C:23]([CH3:24])[C:19]([CH2:18][C:17]3[CH:16]=[CH:15][C:14]([S:11]([CH3:10])(=[O:13])=[O:12])=[CH:27][CH:26]=3)=[C:20]([CH3:21])[C:3]=2[C:4]([OH:9])=[CH:5][CH:6]=1

참가 물질

5

반응물 2

HCID 50700783-Amino-4-chlorophenolHCID 68786995HCID 68786995, 화합물

생성물 1

HCID 136335905HCID 136335905, 화합물

시약·촉매·용매 2

HCID 6395Methanesulfonic Acid촉매HCID 1140Toluene용매

실험 절차

A mixture of 3-amino-4-chlorophenol (1.0 g), 3-(4-methanesulfonylbenzyl)pentane-2,4-dione (0.53 g), methanesulfonic acid (3 drops) and toluene (20 mL) was heated at reflux for 3 hours. The mixture was cooled to room temperature and the solvent removed under reduced pressure. The residue was diluted with ethyl acetate and then washed with water and saturated aqueous sodium chloride solution and dried over magnesium sulfate. The solvent was removed under reduced pressure and purification of the residue by column chromatography on silica gel, eluting with a mixture of dichloromethane and methanol (1:0 to 99:1 by volume) gave title compound as a pale yellow solid, 0.32 g.

후처리

  1. temperaturewas heated
  2. temperatureat reflux for 3 hours
  3. customthe solvent removed under reduced pressure
  4. additionThe residue was diluted with ethyl acetate
  5. washwashed with water and saturated aqueous sodium chloride solution
  6. dry with materialdried over magnesium sulfate
  7. customThe solvent was removed under reduced pressure and purification of the residue by column chromatography on silica gel
  8. washeluting with a mixture of dichloromethane and methanol (1:0 to 99:1 by volume)

출처 및 근거

ORD 기록
ord-ef2fb4552a67418b9ba1bb9ed3b84357
출처 데이터셋
uspto-grants-2010_12
특허 번호
US07858640B2

반응 노트

불러오는 중…