Dabco → HCID 21539297、化合物

HRID 1076227ノート

反応式

HRID 1076227 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.[CH3:17][N:18]=[C:19]=[O:20].N12CCN(CC1)CC2>C1C=CC=CC=1>[CH3:17][NH:18][C:19]([N:14]1[C:15](=[S:16])[C:6]2([CH2:1][CH2:2][CH2:3][CH2:4][CH2:5]2)[NH:7][C:8]21[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9]2)=[O:20]

参加物

5

反応物 3

HCID 9237DabcoHCID 12228Methyl Isocyanate2 回HCID 853997NSC515893

生成物 1

HCID 21539297HCID 21539297、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, 2.28 parts of methyl isocyanate and a trace of 1,4-diazabicyclo[2.2.2]octane in 100 parts of dry benzene were heated at reflux for 4 days. A further 2.28 parts of methyl isocyanate were added and the solution again heated at reflux for 16 hours. The solvent was then evaporated in vacuo and the residue was crystallised twice from ethyl acetate to give 14-methylcarbamoyl-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 4 days
  2. temperaturethe solution again heated
  3. temperatureat reflux for 16 hours
  4. customThe solvent was then evaporated in vacuo
  5. customthe residue was crystallised twice from ethyl acetate

出典と根拠

ORDレコード
ord-ad25879a620b44bdb3012342bd2e4636
出典データセット
uspto-grants-1976_05
特許番号
US03956310

反応ノート

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