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Sulfamic Acid → Ammonia

HRID 617957
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 617957
[NH2:1][C:2]1[N:3]=[CH:4][C:5]2[CH:11]=[C:10]([C:12]3[C:17]([Cl:18])=[CH:16][CH:15]=[CH:14][C:13]=3[Cl:19])[C:9]([NH2:20])=[N:8][C:6]=2[N:7]=1.S(=O)(=O)(O)[NH2:22].[CH2:26]([N:28]([CH2:31][CH2:32]N)[CH2:29][CH3:30])[CH3:27]>>[Cl:19][C:13]1[CH:14]=[CH:15][CH:16]=[C:17]([Cl:18])[C:12]=1[C:10]1[C:9]([NH2:20])=[N:8][C:6]2[N:7]=[C:2]([NH:1][CH2:27][CH2:26][N:28]([CH2:31][CH3:32])[CH2:29][CH3:30])[N:3]=[CH:4][C:5]=2[CH:11]=1.[NH3:22]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 5987Sulfamic AcidHCID 60993N,N-DiethylethylenediamineHCID 53281136-(2,6-Dichlorophenyl)pyrido[2,3-d]pyrimidine-2,7-diamine

Produkt 2

HCID 222AmmoniaAusbeute 1 %HCID 53281286-Arylpyrido[2,3-d]pyrimidine deriv. 26

Reaktionsbedingungen

Temperatur
150 °C

Versuchsvorschrift

A mixture of 2,7-diamino-6-(2,6-dichlorophenyl)-pyrido[2,3-d]pyrimidine (4.0 g) from Example 1, sulfamic acid (2.53 g), and diethylaminoethylamine (40 mL) was heated to approximately 150° C. for 20 hours. The excess diethylaminoethylamine was removed in vacuo. The resulting oil was dissolved in diethyl ether, diluted with hexane, and then filtered. The resulting solid was dissolved in dichloromethane which was washed several times with water, dried with magnesium sulfate, and concentrated in vacuo. The residue was crystallized from ethyl acetate to give the title compound 6-(2, 6-dichlorophenyl)-N2 -(2-diethylaminoethyl)-pyrido[2,3-d]pyrimidine-2,7-diamine, CIMS (1% NH3 in CH4): 433=M+ +C2H5, 405=M+ +H, 389=M+ -Et, 360; mp 216-219.5° C.

Aufarbeitung

  1. customThe excess diethylaminoethylamine was removed in vacuo
  2. dissolutionThe resulting oil was dissolved in diethyl ether
  3. additiondiluted with hexane
  4. filtrationfiltered
  5. dissolutionThe resulting solid was dissolved in dichloromethane which
  6. washwas washed several times with water
  7. dry with materialdried with magnesium sulfate
  8. concentrationconcentrated in vacuo
  9. customThe residue was crystallized from ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-bdfaf0439762485e8efdeb2b7fae8ee4
Quelldatensatz
uspto-grants-1999_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05952342

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