Diisopropylethylamine → [1-(2-Chloro-6,7-dihydrothieno[3,2-d]pyrimidin-4-ylamino)-cyclopropyl]-methanol

HRID 518016Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 518016
[Cl:1][C:2]1[N:3]=[C:4](Cl)[C:5]2[S:10][CH2:9][CH2:8][C:6]=2[N:7]=1.C(N(C(C)C)CC)(C)C.[NH2:21][C:22]1([CH2:25][OH:26])[CH2:24][CH2:23]1>O1CCOCC1>[Cl:1][C:2]1[N:3]=[C:4]([NH:21][C:22]2([CH2:25][OH:26])[CH2:24][CH2:23]2)[C:5]2[S:10][CH2:9][CH2:8][C:6]=2[N:7]=1

Komponenten

5

Edukt 3

HCID 81531DiisopropylethylamineHCID 14146220(1-Aminocyclopropyl)methanolHCID 457899672,4-Dichloro-6,7-dihydrothieno[3,2-d]pyrimidine

Produkt 1

HCID 59708441[1-(2-Chloro-6,7-dihydrothieno[3,2-d]pyrimidin-4-ylamino)-cyclopropyl]-methanol

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel

Reaktionsbedingungen

Temperatur
160 °C

Versuchsvorschrift

1.4 g (II) are placed in 10 ml dioxane, first 3.6 ml diisopropylethylamine, then 1 g of 1-aminocyclopropanemethanol (see 8.2) are added. The reaction mixture is heated to 160° C. until no further reaction takes place, then cooled and evaporated down. The residue is treated with cyclohexane/ethyl acetate (8:2) in the ultrasound bath and the solid is suction filtered and dried. 1.24 g (III-4) are obtained as a solid.

Aufarbeitung

  1. temperaturecooled
  2. customevaporated down
  3. additionThe residue is treated with cyclohexane/ethyl acetate (8:2) in the ultrasound bath
  4. filtrationfiltered
  5. customdried
  6. custom1.24 g (III-4) are obtained as a solid

Quellen und Nachweise

ORD-Eintrag
ord-f116c76b090f4ff19ad93a1953bca5a9
Quelldatensatz
uspto-grants-2015_08
Patentnummer
US09115142B2

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