Triphenylphosphine → HCID 59447602, Verbindung

HRID 1518406

Reaktionsgleichung

Reaktionsgleichung von HRID 1518406
[C:1]([C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[CH:9]=[C:8]([OH:13])[CH:7]=[CH:6]2)#[CH:2].[O:14]1[CH2:19][CH2:18][N:17]([CH2:20][CH2:21][CH2:22]O)[CH2:16][CH2:15]1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.N(/C(OC(C)(C)C)=O)=N\C(OC(C)(C)C)=O>C1COCC1>[C:1]([C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[CH:9]=[C:8]([O:13][CH2:22][CH2:21][CH2:20][N:17]1[CH2:18][CH2:19][O:14][CH2:15][CH2:16]1)[CH:7]=[CH:6]2)#[CH:2]

Komponenten

6

Edukt 4

HCID 11776TriphenylphosphineHCID 1995763-Morpholino-1-propanolHCID 6034084Di-tert-butyl diazene-1,2-dicarboxylateHCID 190817686-Ethynylnaphthalen-2-ol

Produkt 1

HCID 59447602HCID 59447602, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

To a mixture of compound 110B (57 mg, 0.34 mmol), 3-morpholinopropan-1-ol (98 mg, 0.68 mmol) and triphenylphosphine (133 mg, 0.508 mmol) in THF (1.5 ml) was added (E)-di-tert-butyl diazene-1,2-dicarboxylate (117 mg, 0.508 mmol). The reaction mixture was stirred for 1 h and insoluble material was filtered off The filtrate was concentrated and the residue was purified by reverse phase HPLC (gradient: 0-55% acetonitrile in 0.1% TFA water/40 min) to provide compound 110C: LCMS (APCI) 296 (M+H).

Aufarbeitung

  1. filtrationinsoluble material was filtered off The filtrate
  2. concentrationwas concentrated
  3. customthe residue was purified by reverse phase HPLC (gradient: 0-55% acetonitrile in 0.1% TFA water/40 min)

Quellen und Nachweise

ORD-Eintrag
ord-5ef8eb83a00840fab17a22fd983feeda
Quelldatensatz
uspto-grants-2012_07
Patentnummer
US08232273B2

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