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

HRID 2399016노트

반응식

HRID 2399016 반응식
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]

참가 물질

6

반응물 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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d6d913b26305447bad7825424cc6a030
출처 데이터셋
uspto-grants-1977_05
특허 번호
US04026884

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