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Hydrazine, propyl- → HCID 54501544, 화합물

HRID 1447802
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HRID 1447802 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([CH:9]=[C:10]2[C:15](=O)[C:14](=[CH:17][C:18]3[CH:23]=[CH:22][C:21]([O:24][CH3:25])=[CH:20][CH:19]=3)[CH2:13][S:12][CH2:11]2)=[CH:5][CH:4]=1.[CH2:26]([NH:29][NH2:30])[CH2:27][CH3:28]>CO>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([CH:9]2[NH:30][N:29]([CH2:26][CH2:27][CH3:28])[C:15]3[C:14](=[CH:17][C:18]4[CH:23]=[CH:22][C:21]([O:24][CH3:25])=[CH:20][CH:19]=4)[CH2:13][S:12][CH2:11][C:10]2=3)=[CH:5][CH:4]=1
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참가 물질

4

반응물 2

HCID 42007Hydrazine, propyl-HCID 2863313,5-Bis[(4-methoxyphenyl)methylidene]thian-4-one

생성물 1

HCID 54501544HCID 54501544, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A mixture of tetrahydro-3,5-bis-(4-methoxyphenyl-methylene)-4H-thiopyran-4-one (6 g, 17 mmole) and propylhydrazine (1.4 g, 19 mmole) in methanol (250 ml) is heated at reflux temperature for 4.5 hours. After the reaction mixture is left at room temperature overnight, yellow solids precipitate out and are collectd by filtration. The crude product is applied to a Al2O3 column (Activity I, neutral). The major product is eluted with 10-20% ethyl acetate/acetic acid. Continued elution with 10-60% CHCl3 /hexane yields the title compound. Recrystallization from acetone/hexane gives 0.65 g of final product in crystalline form (99% pure), m.p. 131.5°-133.5°.

후처리

  1. temperatureis heated
  2. temperatureat reflux temperature for 4.5 hours
  3. customyellow solids precipitate out and
  4. filtrationare collectd by filtration
  5. washThe major product is eluted with 10-20% ethyl acetate/acetic acid
  6. washContinued elution with 10-60% CHCl3 /hexane

출처 및 근거

ORD 기록
ord-b333823f90cc425395bfc10ce3d7da9b
출처 데이터셋
uspto-grants-1979_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04178379

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