Hydrochloric Acid → HCID 131728370, Verbindung

HRID 2076935Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2076935
O=[C:2]1[CH2:7][O:6][C@H:5]([C:8]2[CH:13]=[C:12]([F:14])[C:11]([F:15])=[CH:10][C:9]=2[F:16])[C@@H:4]([NH:17]C(=O)OCCCC)[CH2:3]1.[F:25][C:26]([F:38])([F:37])[C:27]1[N:28]=[CH:29][C:30]2[CH2:36][CH2:35][NH:34][CH2:33][C:31]=2[N:32]=1.[B][B][B][B][B][B][B][B][B][B].[ClH:49]>CO>[ClH:49].[ClH:49].[F:38][C:26]([F:25])([F:37])[C:27]1[N:28]=[CH:29][C:30]2[CH2:36][CH2:35][N:34]([C@H:2]3[CH2:7][O:6][C@H:5]([C:8]4[CH:13]=[C:12]([F:14])[C:11]([F:15])=[CH:10][C:9]=4[F:16])[C@@H:4]([NH2:17])[CH2:3]3)[CH2:33][C:31]=2[N:32]=1

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 184565172-(Trifluoromethyl)-5,6,7,8-tetrahydropyrido[3,4-d]pyrimidineHCID 131728785HCID 131728785, VerbindungHCID 178419135HCID 178419135, Verbindung

Produkt 1

HCID 131728370HCID 131728370, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel2×

Versuchsvorschrift

To a solution of 45 mg (0.13 mmol) of tent-butyl [(2R,3S)-5-oxo-2-(2,4,5-trifluorophenyl)tetrahydro-2H-pyran-3-yl]carbamate and 27 mg (0.13 mmol) of 2-(trifluoromethyl)-5,6,7,8-tetrahydropyrido[3,4-d]pyrimidine in 2.0 mL of dry methanol was added 5.0 mg (0.039 mmol) of decaborane. The reaction mixture was stirred overnight and concentrated in vacuo, then purified by preparative thin layer chromatography using an Analtech® 1000 micron plate (5% methanol/methylene chloride, 1% concentrated ammonium hydroxide) to give the product which was stirred with hydrochloric acid in methanol (1.3M, 4 mL) for 1 h to give the title product. LC/MS 432.93 (M+1).

Aufarbeitung

  1. concentrationconcentrated in vacuo
  2. custompurified by preparative thin layer chromatography
  3. customto give the product which

Quellen und Nachweise

ORD-Eintrag
ord-2451d8caf0db4fa782f8aca3f7e5a40d
Quelldatensatz
uspto-grants-2011_04
Patentnummer
US07928112B2

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