Potassium Cyanide → HCID 21539321、化合物

HRID 1076228ノート

反応式

HRID 1076228 の反応式
[CH2:1]1[C:6]2([C:15](=[S:16])[NH:14][C:8]3([CH2:13][CH2:12][CH2:11][CH2:10][CH2:9]3)[NH:7]2)[CH2:5][CH2:4][CH2:3][CH2:2]1.[C:17]1([CH3:26])[CH:22]=[CH:21][C:20]([N:23]=[C:24]=[O:25])=[CH:19][CH:18]=1.[C-]#N.[K+].N12CCN(CC1)CC2>C1C=CC=CC=1>[C:17]1([CH3:26])[CH:22]=[CH:21][C:20]([NH:23][C:24]([N:14]2[C:15](=[S:16])[C:6]3([CH2:1][CH2:2][CH2:3][CH2:4][CH2:5]3)[NH:7][C:8]32[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9]3)=[O:25])=[CH:19][CH:18]=1

参加物

6

反応物 4

HCID 9032Potassium CyanideHCID 9237DabcoHCID 693254-Methylphenyl isocyanateHCID 853997NSC515893

生成物 1

HCID 21539321HCID 21539321、化合物

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

4.8 Parts of 7,14-diazadispiro[5.1.5.2]pentadecane-15-thione, 2.92 parts of p-tolyl isocyanate, 0.2 parts of potassium cyanide and a trace of 1,4-diazabicyclo[2.2.2]octane in 100 parts of dry benzene were heated at reflux for 24 hours. The solvent was then evaporated off in vacuo and the residue treated with excess water and allowed to stand for 24 hours. The solution was extracted with chloroform and the axtracts dried and evaporated in vacuo. The residue was crystallised from ethanol to yield 5.4 parts of 14-p-tolylcarbamoyl-7,14-diazadispiro[5.1.5.2]pentadecane-15-thione as a colourless solid of melting point 127° to 129°C. This material gave the following elemental analysis by weight:

後処理

  1. temperatureat reflux for 24 hours
  2. customThe solvent was then evaporated off in vacuo
  3. additionthe residue treated with excess water
  4. extractionThe solution was extracted with chloroform
  5. customthe axtracts dried
  6. customevaporated in vacuo
  7. customThe residue was crystallised from ethanol

出典と根拠

ORDレコード
ord-01e1def291bc435ea14a4c7daabde2c9
出典データセット
uspto-grants-1976_05
特許番号
US03956310

反応ノート

読み込み中…