Ethylenediamine → HCID 10805055、化合物

HRID 649020ノート

反応式

HRID 649020 の反応式
[C:1]([C:3]1[CH:4]=[CH:5][C:6]2[C:7](=[O:19])[C:8]3[C:13]([S:14](=[O:18])(=[O:17])[C:15]=2[CH:16]=1)=[CH:12][CH:11]=[CH:10][CH:9]=3)#[N:2].[CH2:20](N)[CH2:21][NH2:22].C[O-].[Na+]>CO>[NH:2]1[CH2:20][CH2:21][N:22]=[C:1]1[C:3]1[CH:4]=[CH:5][C:6]2[C:7](=[O:19])[C:8]3[C:13]([S:14](=[O:17])(=[O:18])[C:15]=2[CH:16]=1)=[CH:12][CH:11]=[CH:10][CH:9]=3

参加物

5

反応物 3

HCID 3301EthylenediamineHCID 1039579-Oxo-9H-thioxanthene-3-carbonitrile 10,10-dioxideHCID 10942334Sodium Methoxide

生成物 1

HCID 10805055HCID 10805055、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To 13.5 g (0.05 mol) of 3-cyanothioxanthen-9-one 10,10-dioxide was added ethylenediamine, 6.0 g (0.1 mol), and sodium methoxide, 0.5 g (0.01 mol), in 100 ml methanol and the mixture was heated at reflux for 3 days. The reaction mixture was filtered hot and the solid was washed with two 50 ml portions of methanol. The crude product was recrystallized from ethanol to yield 3-(2-imidazolin-2-yl)thioxanthen-9-one 10,10-dioxide, 11.0 g, as bright orange crystals, m.p. 241°-242° C.

後処理

  1. temperatureat reflux for 3 days
  2. filtrationThe reaction mixture was filtered hot
  3. washthe solid was washed with two 50 ml portions of methanol
  4. customThe crude product was recrystallized from ethanol

出典と根拠

ORDレコード
ord-8bf694f09c6343e9b7c0e9e98fcf8f21
出典データセット
uspto-grants-1988_04
特許番号
US04737514

反応ノート

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