Tributylvinyltin → HCID 54101958, Verbindung

HRID 354050

Reaktionsgleichung

[CH2:1]([O:3][P:4]([CH2:9][O:10][C:11]1[CH:16]=[CH:15][C:14](OC)=[CH:13][C:12]=1[N+:19]([O-:21])=[O:20])([O:6][CH2:7][CH3:8])=[O:5])[CH3:2].[CH2:22]([Sn](CCCC)(CCCC)C=C)[CH2:23]CC>CN(C=O)C.[Cl-].[Cl-].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[Pd+2]>[CH2:7]([O:6][P:4]([CH2:9][O:10][C:11]1[CH:16]=[CH:15][C:14]([CH:22]=[CH2:23])=[CH:13][C:12]=1[N+:19]([O-:21])=[O:20])([O:3][CH2:1][CH3:2])=[O:5])[CH3:8]

Komponenten

Reaktionsbedingungen

Temperatur: 60 °C

Versuchsvorschrift

A solution of 2-diethylphosphonomethyloxy-5-bromonitrobenzene (1 mmole, prepared as in Example 37, Step A) in DMF (5 mL) was treated with tributyl(vinyl)tin (1.2 mmole) and palladium bis(triphenylphosphine) dichloride (0.1 mmole), and the mixture was heated at 60° C. under nitrogen for 6 h. Evaporation and chromatography gave 2-diethylphosphonomethyloxy-5-vinylnitrobenzene as an oil which was subjected to Step B of Example 38, Step B of Example 36, and Step D of Example 34 to give 2-amino-7-ethyl-6-thiocyano-4-phosphonomethoxybenzothiazole (41.1). mp >167° C.(dec.). Anal. Calcd. for C11H12N3O4PS2: C:38.26; H:3.50; N:12.17. Found: C:37.87; H:3.47; N: 11.93.

Aufarbeitung

customEvaporation and chromatography

Quellen und Nachweise

ORD-Eintrag: ord-cb46442e978e4c5ea6ef46da9b68f99c
Quelldatensatz: uspto-grants-2004_06
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US06756360B1

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