Dimethylformamide → Methyl 4'-methoxy(1,1'-biphenyl)-4-carboxylate

HRID 1072702

반응식

HRID 1072702 반응식
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:16]=[CH:15][C:11]([C:12](O)=[O:13])=[CH:10][CH:9]=2)=[CH:4][CH:3]=1.IC.CN(C)[CH:21]=[O:22].[C:24](OCC)(=O)C>O>[CH3:24][O:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:16]=[CH:15][C:11]([C:12]([O:22][CH3:21])=[O:13])=[CH:10][CH:9]=2)=[CH:4][CH:3]=1

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 6328Methyl iodideHCID 8857Ethyl AcetateHCID 3015564'-Hydroxy-4-biphenylcarboxylic acid

생성물 1

HCID 1393415Methyl 4'-methoxy(1,1'-biphenyl)-4-carboxylate

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixed solution of 4-(4′-hydroxyphenyl)benzoic acid (10.0 g, 4.67 mmol), iodomethane (19.9 g, 14.0 mmol) and N,N-dimethylformamide (80 ml) was stirred at 60° C. for 3 hours. To the obtained mixture was added ethyl acetate (200 ml) and water (150 ml), the mixture was stirred and the organic layer was separated. The organic layer was washed with 5% aqueous potassium hydrogen sulfate and water, and dried over sodium sulfate anhydride. The solvent was concentrated under reduced pressure and the object compound (10.5 g) was obtained from the residue as colorless crystals. Melting point: 177-178° C.

후처리

  1. customthe organic layer was separated
  2. washThe organic layer was washed with 5% aqueous potassium hydrogen sulfate and water
  3. dry with materialdried over sodium sulfate anhydride
  4. concentrationThe solvent was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-0eed00481a0b48a6bccb4ed8e2a762dd
출처 데이터셋
uspto-grants-2005_06
특허 번호
US06911468B2

연결된 노트

불러오는 중…