Ethylene Glycol → HCID 56626634, 화합물

HRID 1249517노트

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HRID 1249517 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH2:11][CH:12]([N+:25]([O-:27])=[O:26])[CH2:13][CH2:14][C:15](=[O:24])[CH2:16][CH2:17][C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].C1(C)C=CC(S(O)(=O)=O)=CC=1.[CH2:39](O)[CH2:40][OH:41]>C1CCCCC1>[CH2:40]1[O:41][C:15]([CH2:16][CH2:17][C:18]2[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=2)([CH2:14][CH2:13][CH:12]([N+:25]([O-:27])=[O:26])[CH2:11][C:5]2[CH:6]=[CH:7][C:8]([O:9][CH3:10])=[C:3]([O:2][CH3:1])[CH:4]=2)[O:24][CH2:39]1

참가 물질

5

반응물 3

HCID 174Ethylene GlycolHCID 6101p-Toluenesulfonic acidHCID 201642191-(3',4'-Dimethoxyphenyl)-7-phenyl-2-nitro-5-heptanone

생성물 1

HCID 56626634HCID 56626634, 화합물

시약·촉매·용매 1

HCID 8078Cyclohexane용매

실험 절차

Into a 1 l r.b. flask equipped with a Dean Stark trap was placed 46.4 g (0.12 m) of 1-(3',4'-dimethoxyphenyl)-7-phenyl-2-nitro-5-heptanone, 1.5. g p-toluenesulfonic acid, 50 mL of ethylene glycol and 300 mL of cyclohexane. The mixture was allowed to reflux overnight, then concentrated in vacuo. Dil NaHCO3 solution was added to the residue and extracted with ethyl acetate. The organic layer was backwashed with water, dried over anh. MgSO4, filtered and concentrated under reduced pressure to give 45.3 g of an oil which solidified on drying at room temperature under vacuum.

후처리

  1. customflask equipped with a Dean Stark trap
  2. temperatureto reflux overnight
  3. concentrationconcentrated in vacuo
  4. additionDil NaHCO3 solution was added to the residue
  5. extractionextracted with ethyl acetate
  6. dry with materialdried over anh. MgSO4
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-0c578b84a52c48748cece5e6df439487
출처 데이터셋
uspto-grants-1986_12
특허 번호
US04632929

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