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2,5-Dichloropyridine-3-carbonitrile → HCID 67400202、化合物

HRID 914419
ノート
印刷プレビュー

反応式

HRID 914419 の反応式
C([O:5][C:6](=[O:19])[C:7]([S:10][C:11]1[S:12][CH:13]=[C:14]([CH2:16][CH2:17][NH2:18])[N:15]=1)([CH3:9])[CH3:8])(C)(C)C.[Cl:20][C:21]1[N:28]=[CH:27][C:26]([Cl:29])=[CH:25][C:22]=1[C:23]#[N:24].Cl.O1[CH2:36][CH2:35]OCC1>O1CCOCC1>[ClH:20].[Cl:29][C:26]1[CH:25]=[C:22]([C:23]#[N:24])[C:21]([N:18]([CH2:21][CH2:22][CH2:25][CH2:26][CH2:27][CH2:35][CH3:36])[CH2:17][CH2:16][C:14]2[N:15]=[C:11]([S:10][C:7]([CH3:8])([CH3:9])[C:6]([OH:5])=[O:19])[S:12][CH:13]=2)=[N:28][CH:27]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 142116462,5-Dichloropyridine-3-carbonitrileHCID 204431481,4-Dioxane hydrochlorideHCID 597594492-{[4-(2-Aminoethyl)-1,3-thiazol-2-yl]thio}-2-methylpropionic acid tert-butyl ester

生成物 1

HCID 67400202HCID 67400202、化合物

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

A compound obtained by using, as starting materials, 2-{[4-(2-aminoethyl)-1,3-thiazol-2-yl]thio}-2-methylpropionic acid tert-butyl ester synthesized in Example 7 and 2,5-dichloronicotinonitrile synthesized in reference to non-patent reference [Liebigs Ann. Chem., 487, 127 (1931)] and the like, and by operations similar to those of Example 265-1 and Example 265-2, was dissolved in dioxane, an excess amount of 4 mol/L hydrochloric acid-dioxane was added, and the mixture was stirred at room temperature for 12 hr. The reaction mixture was concentrated under reduced pressure, and the residue was purified by silica gel chromatography (elution solvent; chloroform:methanol=10:1) to give the title compound as a colorless oil.

後処理

  1. customA compound obtained
  2. customsynthesized in reference to non-patent reference [Liebigs Ann. Chem., 487, 127 (1931)]
  3. concentrationThe reaction mixture was concentrated under reduced pressure
  4. customthe residue was purified by silica gel chromatography (elution solvent; chloroform:methanol=10:1)

出典と根拠

ORDレコード
ord-455b3f06048042738c27446d6303b276
出典データセット
uspto-grants-2011_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08026370B2

反応ノート

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