Trifluoroacetic acid methylene chloride → HCID 68564037, Verbindung

HRID 970376Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 970376
C(OC([N:8]1[CH2:13][CH2:12][C:11]([NH:18][CH2:19][C:20]2[CH:21]=[CH:22][C:23]3[S:28][CH2:27][C:26](=[O:29])[NH:25][C:24]=3[CH:30]=2)([C:14]([F:17])([F:16])[F:15])[CH2:10][CH2:9]1)=O)(C)(C)C.C(O)(C(F)(F)F)=O.C(Cl)Cl>>[F:16][C:14]([F:15])([F:17])[C:11]1([NH:18][CH2:19][C:20]2[CH:21]=[CH:22][C:23]3[S:28][CH2:27][C:26](=[O:29])[NH:25][C:24]=3[CH:30]=2)[CH2:12][CH2:13][NH:8][CH2:9][CH2:10]1

Komponenten

3

Edukt 2

HCID 21863450Trifluoroacetic acid methylene chlorideHCID 68565409HCID 68565409, Verbindung

Produkt 1

HCID 68564037HCID 68564037, Verbindung

Versuchsvorschrift

A solution of 6-[{1-(tert-butoxycarbonyl)-4-(trifluoromethyl)piperidin-4-ylamino}methyl]-4H-benzo[1,4]thiazin-3-one (3f) in 1:1 TFA/CH2Cl2 is stirred at room temperature until the starting material is consumed, then is concentrated to dryness in vacuo. The residue is partitioned between dilute NaOH and CH2Cl2, and the layers are separated. The aqueous layer is extracted with CH2Cl2, and the combined organic extracts are dried (Na2SO4) and concentrated in vacuo to afford the title compound.

Aufarbeitung

  1. customis consumed
  2. concentrationis concentrated to dryness in vacuo
  3. customThe residue is partitioned between dilute NaOH and CH2Cl2
  4. customthe layers are separated
  5. extractionThe aqueous layer is extracted with CH2Cl2
  6. dry with materialthe combined organic extracts are dried (Na2SO4)
  7. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-2b8063bc6a994faea6b124db82654275
Quelldatensatz
uspto-grants-2007_12
Patentnummer
US07312212B2

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