Triethylamine → HCID 19085347、化合物

HRID 963033

反応式

HRID 963033 の反応式
C1(C)C=CC(S(O)(=O)=O)=CC=1.C1(C)C=CC(S(O)(=O)=O)=CC=1.[NH2:23][CH2:24][C:25]1[N:29]([C:30]2[S:31][C:32]([CH2:44][CH3:45])=[CH:33][C:34]=2[C:35](=[O:43])[C:36]2[CH:41]=[CH:40][CH:39]=[CH:38][C:37]=2[Cl:42])[C:28]([CH3:46])=[N:27][N:26]=1.[Cl:47][C:48]1[CH:53]=[CH:52][CH:51]=[CH:50][C:49]=1[N:54]=[C:55]=[O:56].C(N(CC)CC)C>ClC(Cl)C>[Cl:42][C:37]1[CH:38]=[CH:39][CH:40]=[CH:41][C:36]=1[C:35]([C:34]1[CH:33]=[C:32]([CH2:44][CH3:45])[S:31][C:30]=1[N:29]1[C:28]([CH3:46])=[N:27][N:26]=[C:25]1[CH2:24][NH:23][C:55]([NH:54][C:49]1[CH:50]=[CH:51][CH:52]=[CH:53][C:48]=1[Cl:47])=[O:56])=[O:43]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 76833Chlorophenyl isocyanateHCID 190850953-Aminomethyl-4-(3-(2-chlorobenzoyl)-5-ethylthiophen-2-yl)-5-methyl[1,2,4]triazole ditosylate

生成物 1

HCID 19085347HCID 19085347、化合物

試薬・触媒・溶媒 1

HCID 63651,1-Dichloroethane溶媒

実験手順

3-Aminomethyl-4-(3-(2-chlorobenzoyl)-5-ethylthiophen-2-yl)-5-methyl[1,2,4]triazole di-p-toluenesulfonate (7.40 g) was dissolved in dichloroethane (100 ml). 2-Chlorophenyl isocyanate (1.2 ml) and triethylamine (4.2 ml) were added under ice-cooling, and the mixture was stirred for 4 hours. Then, the reaction mixture was washed with water and dried over magnesium sulfate. The solvent was evaporated, and the residue was purified by silica gel column chromatography (developing solvent:chloroform -methanol) to give 4.50 g of N-(4-(3-(2-chlorobenzoyl)-5-ethylthiophen-2-yl)-5-methyl[1,2,4]triazol-3-ylmethyl)-N'-(2-chlorophenyl)urea as an oil.

後処理

  1. temperaturecooling
  2. washThen, the reaction mixture was washed with water
  3. dry with materialdried over magnesium sulfate
  4. customThe solvent was evaporated
  5. customthe residue was purified by silica gel column chromatography (developing solvent:chloroform -methanol)

出典と根拠

ORDレコード
ord-b080255f100844d992f72484d9ce016e
出典データセット
uspto-grants-1998_06
特許番号
US05760032

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