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

HRID 2179888

反応式

HRID 2179888 の反応式
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]

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid触媒HCID 702Ethanol溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-a9a61f4ca8f04b30a8369b6436cc3cd4
出典データセット
uspto-grants-2005_05
特許番号
US06887867B2

関連ノート

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