Acetohydrazide → 6'-(2-Hydroxypropyl)-4'-methoxy-4-nitrobenzophenone acetylhydrazone

HRID 2179888

반응식

HRID 2179888 반응식
O[C:2]1([C:15]2[CH:20]=[CH:19][C:18]([N+:21]([O-:23])=[O:22])=[CH:17][CH:16]=2)[C:11]2[C:6](=[CH:7][C:8]([O:12][CH3:13])=[CH:9][CH:10]=2)[CH2:5][CH:4]([CH3:14])[O:3]1.[C:24]([NH:27][NH2:28])(=[O:26])[CH3:25]>C(O)C.Cl>[C:24]([NH:27][N:28]=[C:2]([C:11]1[C:6]([CH2:5][CH:4]([OH:3])[CH3:14])=[CH:7][C:8]([O:12][CH3:13])=[CH:9][CH:10]=1)[C:15]1[CH:20]=[CH:19][C:18]([N+:21]([O-:23])=[O:22])=[CH:17][CH:16]=1)(=[O:26])[CH3:25]

참가 물질

5

반응물 2

HCID 14039AcetohydrazideHCID 224889711-Hydroxy-3-methyl-1-(4-nitrophenyl)-6-methoxyisochroman

생성물 1

HCID 865844706'-(2-Hydroxypropyl)-4'-methoxy-4-nitrobenzophenone acetylhydrazone수율 66.3%

시약·촉매·용매 2

HCID 313Hydrochloric Acid촉매HCID 702Ethanol용매

실험 절차

To a solution of 4 (1.6 g) in 25 ml of ethanol was added acetic hydrazide (0.4 g) and 2 drops of concentrated HCl. The resulting solution was heated to reflux for 3 hours. The solvent was removed under reduced pressure. The residue was treated with NaHCO3, and extracted with ethyl acetate. The combined organic phase was washed with brine, dried over Na2SO4. Removal of the solvent gave the desired product (1.25 g).

후처리

  1. temperatureThe resulting solution was heated
  2. temperatureto reflux for 3 hours
  3. customThe solvent was removed under reduced pressure
  4. additionThe residue was treated with NaHCO3
  5. extractionextracted with ethyl acetate
  6. washThe combined organic phase was washed with brine
  7. dry with materialdried over Na2SO4
  8. customRemoval of the solvent

출처 및 근거

ORD 기록
ord-a9a61f4ca8f04b30a8369b6436cc3cd4
출처 데이터셋
uspto-grants-2005_05
특허 번호
US06887867B2

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