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Water → HCID 68124900、化合物

HRID 596776
ノート
印刷プレビュー

反応式

HRID 596776 の反応式
[CH:1](/[C:9]1[N:13]=[CH:12][O:11][N:10]=1)=[CH:2]\[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.O>C(O)C.[Hg]>[CH:1](/[C:9]1[N:13]=[CH:12][O:11][N:10]=1)=[CH:2]/[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 962WaterHCID 64414463-[(E)-2-Phenylethen-1-yl]-1,2,4-oxadiazole

生成物 1

HCID 68124900HCID 68124900、化合物

試薬・触媒・溶媒 2

HCID 23931Mercury触媒HCID 702Ethanol溶媒

実験手順

3-(trans-Styryl)-1,2,4-oxadiazole (0.75 g.) in absolute ethanol (750 ml.) was irradiated at room temperature, under nitrogen for a total of 31 hr. using a medium pressure mercury vapour arc tube contained in a water cooled glass well immersed in the solution. The ultraviolet spectra of suitably diluted aliquots showed a reduction in the intensity of absorption at ca. 274 nm over the period of irradiation. The colourless solution was evaporated to a low volume when the trans isomer (0.11 g.), m.p. 84° , λmax. (EtOH) 274 nm (ε 26,200) separated. Evaporation of the mother liquors to dryness gave a solid and an oil. The oil was separated and thoroughly dried to give 3-(cis-styryl)-1,2,4-oxadiazole contaminated with ca. 25% by weight of the trans-isomer, λmax. (EtOH) 272-273 nm (ε 14,300), pmr. shows cis-protons at 2.92 and 3.50 (J = 12.5) and confirms the presence of the transisomer.

後処理

  1. customin the intensity of absorption at ca. 274 nm
  2. customover the period of irradiation
  3. customThe colourless solution was evaporated to a low volume when the trans isomer (0.11 g.), m.p. 84° , λmax
  4. custom(EtOH) 274 nm (ε 26,200) separated
  5. customEvaporation of the mother liquors to dryness
  6. customgave a solid
  7. customThe oil was separated
  8. customthoroughly dried

出典と根拠

ORDレコード
ord-43af3e5173a24e8bb83a34ed8d864bed
出典データセット
uspto-grants-1977_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04012377

反応ノート

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