2-Pyridinyl-1,3-dioxolane → 1-(2,5-Dibromobenzyl)-2-(1,3-dioxolan-2-yl)pyridinium bromide

HRID 742476

반응식

HRID 742476 반응식
[O:1]1[CH2:5][CH2:4][O:3][CH:2]1[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][N:7]=1.[Br:12][C:13]1[CH:20]=[CH:19][C:18]([Br:21])=[CH:17][C:14]=1[CH2:15]Br>S1(CCCC1)(=O)=O.C(OCC)(=O)C>[Br-:12].[Br:12][C:13]1[CH:20]=[CH:19][C:18]([Br:21])=[CH:17][C:14]=1[CH2:15][N+:7]1[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=1[CH:2]1[O:3][CH2:4][CH2:5][O:1]1

참가 물질

5

반응물 2

HCID 797732-Pyridinyl-1,3-dioxolaneHCID 53260381,4-Dibromo-2-(bromomethyl)benzene

생성물 1

HCID 190475031-(2,5-Dibromobenzyl)-2-(1,3-dioxolan-2-yl)pyridinium bromide수율 157.2%

시약·촉매·용매 2

HCID 8857Ethyl Acetate용매HCID 31347Sulfolane용매

실험 절차

A mixture of 25.03 g (0.165 mol) of 2-(1,3-dioxolan-2-yl)pyridine and 2,5-dibromobenzyl bromide (54 g, 0.165 mol) in 60 mL of sulfolane was heated on a steam-bath for 6 h. The mixture was diluted with 600 mL of ethyl acetate, cooled, and the resulting solid product was isolated by filtration. The above solid was triturated in 300 mL of ethyl acetate, the mixture was cooled, filtered and dried to afford 62.24 g (79%) of 1-(2,5-dibromobenzyl)-2-(1,3-dioxolan-2-yl)pyridinium bromide (Formula VI: R1 =R2 =H; R7 =2,5-Br2 ; Z- =Br-), as a yellow solid, m.p. 135°-139° C.

후처리

  1. temperaturewas heated on a steam-bath for 6 h
  2. temperaturecooled
  3. customthe resulting solid product was isolated by filtration
  4. customThe above solid was triturated in 300 mL of ethyl acetate
  5. temperaturethe mixture was cooled
  6. filtrationfiltered
  7. customdried

출처 및 근거

ORD 기록
ord-765e1ed5c3214074bbde20da683aad41
출처 데이터셋
uspto-grants-1996_09
특허 번호
US05554620

연결된 노트

불러오는 중…