Acetophenone → Acetophenone benzoylhydrazone

HRID 22098

반응식

HRID 22098 반응식
[C:1]([NH:9][NH2:10])(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:11]([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)(=O)[CH3:12]>O1CCCC1>[C:1]([NH:9][N:10]=[C:11]([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)[CH3:12])(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

4

반응물 2

HCID 7410AcetophenoneHCID 11955Benzoylhydrazine

생성물 1

HCID 346107Acetophenone benzoylhydrazone

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
25 °C

실험 절차

To a solution of benzoic acid hydrazide (5.70 g, 0.042 mol) in tetrahydrofuran (75 mL) was added acetophenone (5.5 g, 0.046 mol) followed by concentrated. HCl (3 drops). The reaction was allowed to stir for 12 h at 25° C. during which time the product precipitated as a colorless crystalline solid. The product was filtered, washed with tetrahydrofuran (1×30 mL), diethyl ether (3×60 mL) and pentane (2×60 mL), and the crystalline solids were dried in vacuo (6.65 g, 64%). 1H NMR (CD2Cl2): δ2.35 (s, 3H, CH3), 7.30-8.0 (m, 10H, Ph), 9.0 (br, 1H, NH). All other substrates were prepared in a similar fashion.

후처리

  1. concentrationby concentrated
  2. customprecipitated as a colorless crystalline solid
  3. filtrationThe product was filtered
  4. washwashed with tetrahydrofuran (1×30 mL), diethyl ether (3×60 mL) and pentane (2×60 mL)
  5. customthe crystalline solids were dried in vacuo (6.65 g, 64%)
  6. customAll other substrates were prepared in a similar fashion

출처 및 근거

ORD 기록
ord-0b866c1b184048648795054c228cf6bd
출처 데이터셋
uspto-grants-1995_06
특허 번호
US05426223

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