Sodium Bicarbonate → HCID 67498868, Verbindung

HRID 74265Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 74265
[F:1][C:2]([F:23])([F:22])[CH2:3][CH2:4][NH:5][C:6]1[CH:12]=[CH:11][C:10]([C:13]2[O:14][C:15]3[CH:21]=[CH:20][CH:19]=[CH:18][C:16]=3[N:17]=2)=[CH:9][C:7]=1[NH2:8].Cl.[C:25](=N)(OC)[CH3:26].C(=O)([O-])O.[Na+]>CO>[O:14]1[C:15]2[CH:21]=[CH:20][CH:19]=[CH:18][C:16]=2[N:17]=[C:13]1[C:10]1[CH:11]=[CH:12][C:6]2[N:5]([CH2:4][CH2:3][C:2]([F:1])([F:22])[F:23])[C:25]([CH3:26])=[N:8][C:7]=2[CH:9]=1

Komponenten

5

Edukt 3

HCID 516892Sodium BicarbonateHCID 10313100Ethanimidic acid, methyl ester, hydrochloride (1:1)HCID 674986742-(2-(3,3,3-Trifluoropropyl)aminoanilin-5-yl)benzoxazole

Produkt 1

HCID 67498868HCID 67498868, VerbindungAusbeute 93 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

To a methanol (5 mL) solution of 2-(2-(3,3,3-trifluoropropyl)aminoanilin-5-yl)benzoxazole (see Working Example 85-1) (300 mg, 0.93 mmol) was added methyl acetimidate hydrochloride (120 mg, 1.11 mmol), and this was heated to reflux for 3 hours. After the reaction was complete, saturated aqueous sodium hydrogen carbonate solution was added, and this was extracted with chloroform. The organic layer obtained was dried over anhydrous sodium sulfate, after which it was filtered and concentrated to yield the title compound (250 mg, 93% yield) as white crystals.

Aufarbeitung

  1. temperaturethis was heated
  2. temperatureto reflux for 3 hours
  3. extractionthis was extracted with chloroform
  4. customThe organic layer obtained
  5. dry with materialwas dried over anhydrous sodium sulfate
  6. filtrationafter which it was filtered
  7. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-0f8615389ce341508bbf451608ecf06d
Quelldatensatz
uspto-grants-2014_09
Patentnummer
US08829035B2

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