Water → 1,3-Diethyl-5-{bis[(1,3-diethyl-1H-imidazo[4,5-b]quinoxalin-2-(3H)-ylidene)methyl]methylene}-2-thiobarbituric acid

HRID 2399016ノート

反応式

HRID 2399016 の反応式
Cl([O-])(=O)(=O)=O.[CH2:6]([N+:8]1[C:12]2=[N:13][C:14]3[C:19]([N:20]=[C:11]2[N:10]([CH2:21][CH3:22])[C:9]=1[C:23]#[C:24][CH:25]=[C:26]1[N:38]([CH2:39][CH3:40])[C:29]2=[N:30][C:31]4[C:36]([N:37]=[C:28]2[N:27]1[CH2:41][CH3:42])=[CH:35][CH:34]=[CH:33][CH:32]=4)=[CH:18][CH:17]=[CH:16][CH:15]=3)[CH3:7].[CH2:43]([N:45]1[C:52](=[O:53])[CH2:51][C:49](=[O:50])[N:48]([CH2:54][CH3:55])[C:46]1=[S:47])[CH3:44].C(N(CC)CC)C.O>CN(C)C=O>[CH2:54]([N:48]1[C:49](=[O:50])[C:51](=[C:24]([CH:25]=[C:26]2[N:27]([CH2:41][CH3:42])[C:28]3=[N:37][C:36]4[C:31]([N:30]=[C:29]3[N:38]2[CH2:39][CH3:40])=[CH:32][CH:33]=[CH:34][CH:35]=4)[CH:23]=[C:9]2[N:10]([CH2:21][CH3:22])[C:11]3=[N:20][C:19]4[C:14]([N:13]=[C:12]3[N:8]2[CH2:6][CH3:7])=[CH:15][CH:16]=[CH:17][CH:18]=4)[C:52](=[O:53])[N:45]([CH2:43][CH3:44])[C:46]1=[S:47])[CH3:55]

参加物

6

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 788901,3-Diethyl-2-thiobarbituric acidHCID 867347981,3-diethyl-2-[(1,3-diethyl-1H-imidazo[4,5-b]quinoxalin-2-(3H)-ylidene)-1-propynyl]imidazo[4,5-b]quinoxalinium perchlorate

生成物 1

HCID 203629651,3-Diethyl-5-{bis[(1,3-diethyl-1H-imidazo[4,5-b]quinoxalin-2-(3H)-ylidene)methyl]methylene}-2-thiobarbituric acid

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 1,3-diethyl-2-[(1,3-diethyl-1H-imidazo[4,5-b]quinoxalin-2-(3H)-ylidene)-1-propynyl]imidazo[4,5-b]quinoxalinium perchlorate) 0.33 g, 0.0005 mol) of Example 1, 1,3-diethyl-2-thiobarbituric acid (0.11 g, 0.0005 mol) and triethylamine (0.10 g, 0.001 mol) in dimethylformamide (5 ml), is heated at reflux for 30 seconds. After cooling the solution is diluted to 20 ml. with water. The dye is collected and washed with water. After recrystallization from acetonitrile, the yield of purified dye is 0.27 g (79%) - mp. indistinct.

後処理

  1. temperatureis heated
  2. temperatureat reflux for 30 seconds
  3. temperatureAfter cooling the solution
  4. additionis diluted to 20 ml
  5. customThe dye is collected
  6. washwashed with water
  7. customAfter recrystallization from acetonitrile

出典と根拠

ORDレコード
ord-d6d913b26305447bad7825424cc6a030
出典データセット
uspto-grants-1977_05
特許番号
US04026884

反応ノート

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