O-Phenylenediamine → ethyl 2-(1H-1,3-benzodiazol-2-yl)acetate

HRID 353787

反応式

HRID 353787 の反応式
[C:1]1([NH2:8])[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[NH2:7].Cl.C(O[C:13](=N)[CH2:14][C:15]([O:17][CH2:18][CH3:19])=[O:16])C>CCO>[N:7]1[C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][C:1]=2[NH:8][C:13]=1[CH2:14][C:15]([O:17][CH2:18][CH3:19])=[O:16]

参加物

4

反応物 2

HCID 7243O-PhenylenediamineHCID 75345Ethyl 3-ethoxy-3-iminopropionate hydrochloride

生成物 1

HCID 308071ethyl 2-(1H-1,3-benzodiazol-2-yl)acetate

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of 1,2-phenylenediamine (1.0 eq) and ethyl 3-ethoxy-3-iminopropanoate hydrochloride (1.3 eq) in EtOH was stirred at 90° C. overnight. The reaction was cooled to room temperature and the solvent removed in vacuo. Water and CH2Cl2 were added to the residue. The organic layer was separated, dried over Na2SO4 and the solvent removed. The solid recovered was used without purification. LC/MS m/z 205.2 (MH+), Rt 1.44 minutes.

後処理

  1. customthe solvent removed in vacuo
  2. additionWater and CH2Cl2 were added to the residue
  3. customThe organic layer was separated
  4. dry with materialdried over Na2SO4
  5. customthe solvent removed
  6. customThe solid recovered
  7. customwas used without purification

出典と根拠

ORDレコード
ord-7ebd6310aecc423cba1434ab8eef2675
出典データセット
uspto-grants-2004_06
特許番号
US06756383B2

関連ノート

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