Hydrazine, propyl- → HCID 53955405、化合物

HRID 1576022ノート

反応式

HRID 1576022 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:9]=[C:10]2[C:15](=O)[C:14](=[CH:17][C:18]3[CH:23]=[CH:22][C:21]([Cl:24])=[C:20]([Cl:25])[CH:19]=3)[CH2:13][S:12][CH2:11]2)[CH:5]=[CH:6][C:7]=1[Cl:8].[CH2:26]([NH:29][NH2:30])[CH2:27][CH3:28]>CO.C(Cl)(Cl)Cl>[Cl:1][C:2]1[CH:3]=[C:4]([CH:9]2[N:29]([CH2:26][CH2:27][CH3:28])[N:30]=[C:15]3[C:14](=[CH:17][C:18]4[CH:23]=[CH:22][C:21]([Cl:24])=[C:20]([Cl:25])[CH:19]=4)[CH2:13][S:12][CH2:11][CH:10]23)[CH:5]=[CH:6][C:7]=1[Cl:8]

参加物

4

反応物 2

HCID 42007Hydrazine, propyl-HCID 5149244H-Thiopyran-4-one, 3,5-bis[(3,4-dichlorophenyl)methylene]tetrahydro-

生成物 1

HCID 53955405HCID 53955405、化合物

試薬・触媒・溶媒 1

HCID 21584188Chloroform methanol溶媒

実験手順

A suspension of 6.5g of tetrahydro-3,5-bis-[(3,4-dichlorophenyl)methylene]-4H-thiopyran-4-one and 1.1g of n-propyl hydrazine in 250ml of methanol/chloroform (1:1) is heated at reflux temperature for about 16 hours. The reaction mixture is allowed to cool slightly. Unreacted starting material precipitates out and is removed by filtration. The filtrate is concentrated in vacuo, added to chloroform and washed with dilute hydrochloric acid and water. The organic layer is dried with magnesium sulfate and concentrated in vacuo to 5g of a semi-solid material. This is applied to a wet-packed (hexane) neutral alumina column (Activity I) and eluted with 0-100% ether/hexane. Elution with 10-40% ether/hexane yields the product as an oil.

後処理

  1. temperatureis heated
  2. temperatureat reflux temperature for about 16 hours
  3. temperatureto cool slightly
  4. customprecipitates out and
  5. customis removed by filtration
  6. concentrationThe filtrate is concentrated in vacuo
  7. additionadded to chloroform
  8. washwashed with dilute hydrochloric acid and water
  9. dry with materialThe organic layer is dried with magnesium sulfate
  10. concentrationconcentrated in vacuo to 5g of a semi-solid material
  11. washeluted with 0-100% ether/hexane
  12. washElution with 10-40% ether/hexane

出典と根拠

ORDレコード
ord-53165c105d484d6daa35662fa3809940
出典データセット
uspto-grants-1976_09
特許番号
US03979381

反応ノート

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