2-Butanamine, 2-methyl- → 3-(Tert-amylamino)-4-(2-hydroxy-6-cyanophenyl)amino-3-cyclobutene-1,2-dione

HRID 357295

Reaktionsgleichung

Reaktionsgleichung von HRID 357295
C(O[C:4]1[C:5](=[O:19])[C:6](=[O:18])[C:7]=1[NH:8][C:9]1[C:14]([C:15]#[N:16])=[CH:13][CH:12]=[CH:11][C:10]=1[OH:17])C.[C:20]([NH2:25])([CH2:23][CH3:24])([CH3:22])[CH3:21]>C(Cl)Cl>[C:20]([NH:25][C:4]1[C:5](=[O:19])[C:6](=[O:18])[C:7]=1[NH:8][C:9]1[C:14]([C:15]#[N:16])=[CH:13][CH:12]=[CH:11][C:10]=1[OH:17])([CH2:23][CH3:24])([CH3:22])[CH3:21]

Komponenten

4

Edukt 2

HCID 689862-Butanamine, 2-methyl-HCID 111187243-Ethoxy-4-(2-hydroxy-6-cyanophenyl)amino-3-cyclobutene-1,2-dione

Produkt 1

HCID 99262963-(Tert-amylamino)-4-(2-hydroxy-6-cyanophenyl)amino-3-cyclobutene-1,2-dione

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

A mixture of 3-ethoxy-4-(2-hydroxy-6-cyanophenyl)amino-3-cyclobutene-1,2-dione (0.250 g, 0.00097 mol) and tert-amylamine (1.13 ml, 0.0097 mol) was stirred in enough CH2Cl2 to form a solution at room temperature for two days. During this time a precipitate forms. The reaction solvent is evaporated on a rotary evaporator, the residue is taken up in ethyl acetate and extracted well with 0.25N HCl. The organic layer is washed once with distilled water, dried (Na2SO4), and evaporated to a solid. The solid is collected and gives 3-(tert-amylamino)-4-(2-hydroxy-6-cyanophenyl)amino-3-cyclobutene-1,2-dione, 0.135 g (0.00045 mol, 46%).

Aufarbeitung

  1. customto form a solution at room temperature for two days
  2. customThe reaction solvent is evaporated on a rotary evaporator
  3. extractionextracted well with 0.25N HCl
  4. washThe organic layer is washed once with distilled water
  5. dry with materialdried (Na2SO4)
  6. customevaporated to a solid
  7. customThe solid is collected

Quellen und Nachweise

ORD-Eintrag
ord-5fb74f62d69c4b8c979ef3bbd60ab2ac
Quelldatensatz
uspto-grants-1998_11
Patentnummer
US05840764

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