Methylamine → 5-(2-Methylaminoethoxy)benzofurazan hydrobromide

HRID 1195680ノート

反応式

HRID 1195680 の反応式
[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

参加物

4

反応物 2

HCID 6329MethylamineHCID 190453515-(2-Bromoethoxy)benzofurazan

生成物 1

HCID 679164435-(2-Methylaminoethoxy)benzofurazan hydrobromide収率 81%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-7fb04d32d9d24b9cbaf05485b35f3a9d
出典データセット
uspto-grants-1992_05
特許番号
US05112824

反応ノート

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