Sodium → HCID 13236222、化合物

HRID 462691ノート

反応式

HRID 462691 の反応式
[Na].[OH:2][C:3]1(C2C=CC=CC=2)[NH:7][C:6](=[S:8])[C:5]([C:9]#[N:10])=[C:4]1[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1>C(O)C>[C:11]1([C:4]2([C:11]3[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=3)[C:3](=[O:2])[NH:7][C:6]([S:8][CH:4]([CH3:3])[CH2:5][CH3:6])=[C:5]2[C:9]#[N:10])[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1

参加物

4

反応物 2

HCID 5360545SodiumHCID 132361755-Hydroxy-4,5-diphenyl-2-sulfanylidene-2,5-dihydro-1H-pyrrole-3-carbonitrile

生成物 1

HCID 13236222HCID 13236222、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

0.8 g. Sodium is dissolved in 150 ml. absolute ethanol, 10.0 g. 5-hydroxy-4,5-diphenyl-2-thioxo-3-pyrroline-3-carbonitrile are added thereto and the reaction mixture is boiled for 30 minutes. The solvent is thereafter removed on a rotary evaporator and the residue is taken up in 100 ml. dimethylformamide. 5.1 g. sec.-Butyl bromide are added thereto, the reaction mixture is stirred for 24 hours at ambient temperature, a further 3.0 g. of the alkylating agent are again added thereto and stirring is continued for 24 hours. Thereafter, the solvent is distilled off under wafter pump vacuum and the residue is triturated with water. The precipitate is filtered off with suction, washed with water and crystallised from ethanol. There are obtained 7.0 g. of the desired product in the form of colourless crystals; m.p. 155°-156° C.

後処理

  1. customThe solvent is thereafter removed on a rotary evaporator
  2. additionsec.-Butyl bromide are added
  3. additionof the alkylating agent are again added
  4. stirringstirring
  5. waitis continued for 24 hours
  6. distillationThereafter, the solvent is distilled off under wafter pump vacuum
  7. customthe residue is triturated with water
  8. filtrationThe precipitate is filtered off with suction
  9. washwashed with water
  10. customcrystallised from ethanol
  11. customThere are obtained 7.0 g

出典と根拠

ORDレコード
ord-20371b2b45c04fa1a7077b041cc71ff2
出典データセット
uspto-grants-1985_05
特許番号
US04517185

反応ノート

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