Methylamine → 5-(2-Methylaminoethoxy)benzofurazan hydrobromide

HRID 1195680노트

반응식

HRID 1195680 반응식
[Br:1][CH2:2][CH2:3][O:4][C:5]1[CH:6]=[CH:7][C:8]2[C:9]([CH:13]=1)=[N:10][O:11][N:12]=2.[CH3:14][NH2:15]>C(O)C>[BrH:1].[CH3:14][NH:15][CH2:2][CH2:3][O:4][C:5]1[CH:6]=[CH:7][C:8]2[C:9]([CH:13]=1)=[N:10][O:11][N:12]=2

참가 물질

4

반응물 2

HCID 6329MethylamineHCID 190453515-(2-Bromoethoxy)benzofurazan

생성물 1

HCID 679164435-(2-Methylaminoethoxy)benzofurazan hydrobromide수율 81%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a solution of 5-(2-bromoethoxy)benzofurazan (0.84 g, 3.4 mmol) in ethanol (45 ml), contained within a Fisher-Porter pressure vessel cooled with ice/acetone was added methylamine (45 ml). The vessel was sealed, the bath removed and the solution was stirred at room temperature overnight. The reaction mixture was concentrated under reduced pressure and the residue flushed with ethanol. Recrystallization from ethyl acetate-hexane gave 5-(2-methylaminoethoxy)benzofurazan hydrobromide (0.75 g, 81%); 1H NMR (DMSO) δ2.68 (s, 3H), 3.45 (t, 2H), 4.43 (t, 2H), 7.34 (m, 2H), 8.04 (d, 1H, J=9.6 Hz), 8.76 (bs, 2H).

후처리

  1. customThe vessel was sealed
  2. customthe bath removed
  3. concentrationThe reaction mixture was concentrated under reduced pressure
  4. customthe residue flushed with ethanol
  5. customRecrystallization from ethyl acetate-hexane

출처 및 근거

ORD 기록
ord-7fb04d32d9d24b9cbaf05485b35f3a9d
출처 데이터셋
uspto-grants-1992_05
특허 번호
US05112824

반응 노트

불러오는 중…