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Carbon Disulfide → HCID 19979372、化合物

HRID 1461767
ノート
印刷プレビュー

反応式

HRID 1461767 の反応式
C(N(CC)CC)C.[C:8](=[S:10])=S.[CH:11]([C:14]1[C:19]([NH2:20])=[C:18]([CH:21]([CH3:23])[CH3:22])[CH:17]=[C:16]([O:24][C:25]2[CH:30]=[CH:29][C:28]([Cl:31])=[CH:27][CH:26]=2)[N:15]=1)([CH3:13])[CH3:12].C1(N=C=NC2CCCCC2)CCCCC1>N1C=CC=CC=1>[CH:11]([C:14]1[C:19]([N:20]=[C:8]=[S:10])=[C:18]([CH:21]([CH3:23])[CH3:22])[CH:17]=[C:16]([O:24][C:25]2[CH:30]=[CH:29][C:28]([Cl:31])=[CH:27][CH:26]=2)[N:15]=1)([CH3:12])[CH3:13]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6348Carbon DisulfideHCID 8471TriethylamineHCID 10868DicyclohexylcarbodiimideHCID 19979371HCID 19979371、化合物

生成物 1

HCID 19979372HCID 19979372、化合物

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒3 回

反応条件

温度
-10 °C

実験手順

A solution of 5.0 g of triethylamine in 10 ml of pyridine is cooled to from -5° C. to -10° C., and 20 ml of carbon disulfide are added dropwise. At -10° C., a solution of 15.0 g of 2,4-diisopropyl-6-(4-chlorophenoxy)-3-aminopyridine in 27 ml of pyridine is slowly added dropwise. The mixture is further stirred at -10° C. for 1 hour. A solution of 10.0 g of N,N'-dicyclohexylcarbodiimide in 10 ml of pyridine is then added. After a further 3 hours at -10° C., the mixture is stirred for 18 hours at room temperature. The reaction mixture is concentrated by evaporation and hexane is added to the residue. Thehhexane solution is filtered off and concentrated by evaporation. 2,4-Diisopropyl-6-(4-chlorophenoxy)-pyrid-3-yl isothiocyanate is obtained in the form of a yellow oil, which is used for the next reaction without being further purified; IR (CCl 4): 2090, 1490, 1220 cm-1.

後処理

  1. additionare added dropwise
  2. waitAfter a further 3 hours at -10° C.
  3. stirringthe mixture is stirred for 18 hours at room temperature
  4. concentrationThe reaction mixture is concentrated by evaporation and hexane
  5. additionis added to the residue
  6. filtrationThehhexane solution is filtered off
  7. concentrationconcentrated by evaporation

出典と根拠

ORDレコード
ord-7a5ca98f2e1141928f89b024ff66ffcb
出典データセット
uspto-grants-1991_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05077304

反応ノート

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