p-Anisoyl chloride → Methanone, (5-bromo-2-thienyl)(4-methoxyphenyl)-

HRID 1153786노트

반응식

HRID 1153786 반응식
[Br:1][C:2]1[S:3][CH:4]=[CH:5][CH:6]=1.[CH3:7][O:8][C:9]1[CH:17]=[CH:16][C:12]([C:13](Cl)=[O:14])=[CH:11][CH:10]=1>C(Cl)Cl>[Br:1][C:2]1[S:3][C:4]([C:13](=[O:14])[C:12]2[CH:16]=[CH:17][C:9]([O:8][CH3:7])=[CH:10][CH:11]=2)=[CH:5][CH:6]=1

참가 물질

4

반응물 2

HCID 7477p-Anisoyl chlorideHCID 138512-Bromothiophene

생성물 1

HCID 298606Methanone, (5-bromo-2-thienyl)(4-methoxyphenyl)-

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a cold (0°-5° C.) solution of 2-bromothiophene (32.6 g, 0.2 mol) and p-methoxybenzoyl chloride (34.1 g, 0.2 mol) in methylene chloride was added anhydrous stannic chloride (52 g, 0.2 mol) dropwise over about one hour. When addition was complete, the cooling bath was removed and the solution was stirred for an additional two hours. A solution of water (90 mL) and concentrated hydrochloric acid (10 mL) was added dropwise and the layers were separated. The organic layer was washed with water, saturated sodium chloride solution and dried (MgSO4). Removal of the solvent in vacuo and collection of the slide with the aid of hexane gave 48.5 g, of gray powder, m.p. 97°-99° C. A sample was recrystallized from ligroin for analysis.

후처리

  1. additionWhen addition
  2. customthe cooling bath was removed
  3. additionA solution of water (90 mL) and concentrated hydrochloric acid (10 mL) was added dropwise
  4. customthe layers were separated
  5. washThe organic layer was washed with water, saturated sodium chloride solution
  6. dry with materialdried (MgSO4)
  7. customRemoval of the solvent
  8. customin vacuo and collection of the slide with the aid of hexane
  9. customgave 48.5 g
  10. customA sample was recrystallized from ligroin for analysis

출처 및 근거

ORD 기록
ord-e7157db65c4645a895023c98da45370a
출처 데이터셋
uspto-grants-1984_12
특허 번호
US04486444

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