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

HRID 392607

반응식

HRID 392607 반응식
[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>C(O)C>[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A solution of 1,2-phenylenediamine (1.0 eq) and ethyl 3-ethoxy-3-iminopropanoate hydrochloride (1.3 eq) in ethanol was stirred at 90° C. overnight. The reaction was cooled to room temperature and the solvent was 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+), Rf 1.44 minutes.

후처리

  1. customthe solvent was 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

출처 및 근거

ORD 기록
ord-0a0a45617ce141bc9ed3ed9c77d5f347
출처 데이터셋
uspto-grants-2004_10
특허 번호
US06800760B2

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