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2-Chlorobenzaldehyde → HCID 13564978, 화합물

HRID 236571
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HRID 236571 반응식
[Cl:1][C:2]1[CH:9]=[CH:8][CH:7]=[CH:6][C:3]=1[CH:4]=O.[NH2:10]/[C:11](/[CH3:22])=[CH:12]\[C:13]([O:15][CH2:16][CH2:17][O:18][C:19](=[O:21])[CH3:20])=[O:14].[N+:23]([CH2:26][C:27](=O)[CH3:28])([O-:25])=[O:24]>C(O)C>[CH3:28][C:27]1[NH:10][C:11]([CH3:22])=[C:12]([C:13]([O:15][CH2:16][CH2:17][O:18][C:19](=[O:21])[CH3:20])=[O:14])[CH:4]([C:3]2[CH:6]=[CH:7][CH:8]=[CH:9][C:2]=2[Cl:1])[C:26]=1[N+:23]([O-:25])=[O:24]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 69962-ChlorobenzaldehydeHCID 662962-Propanone, 1-nitro-HCID 21278157HCID 21278157, 화합물

생성물 1

HCID 13564978HCID 13564978, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

28.1 g (200 mmol) of 2-chlorobenzaldehyde are boiled under reflux with 37.4 g (200 mmol) of 2-acetoxyethyl β-aminocrotonate and 32.6 g (320 mmol) of nitroacetone in 400 ml of ethanol for 4 hours. The mixture is cooled and concentrated. The evaporation residue is taken up in ethyl acetate and the mixture is washed with water, sodium bicarbonate solution and water again, dried and concentrated. The semi-solid evaporation residue is stirred with ethanol, filtered off with suction and washed with ethanol. 23.2 g (29.4% of theory) of a yellow-colored product of melting point 158°-160° C. are obtained.

후처리

  1. temperatureThe mixture is cooled
  2. concentrationconcentrated
  3. washthe mixture is washed with water, sodium bicarbonate solution and water again
  4. customdried
  5. concentrationconcentrated
  6. customThe semi-solid evaporation residue
  7. filtrationfiltered off with suction
  8. washwashed with ethanol
  9. custom23.2 g (29.4% of theory) of a yellow-colored product of melting point 158°-160° C. are obtained

출처 및 근거

ORD 기록
ord-09dfd876ef0a4019949835f7b55cc85e
출처 데이터셋
uspto-grants-1987_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04645775

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