+++Поиск по Reaxys_Спасибо

[paramona]

Доброе!
Я конечно дико извиняюсь.

Коллеги, проведите, пожалуйста, поиск по приведенным структурам (получение и физ. хим. свойства), и если эти соединения описано, то где конкретно.

1) CC(C)(C)OC(=O)COCCOCCOCC(=O)OC(C)(C)C

2) O=C(COCCOCCOCC(=O)OCc1ccccc1)OCc2ccccc2

Заранее благодарен.

[mishka]

O=C(COCCOCCOCC(=O)OCc1ccccc1)OCc2ccccc2
вообще нет

для другого есть ямр

Description (NMR Spectroscopy) Nucleus (NMR Spectroscopy) Solvents (NMR Spectroscopy) Frequency (NMR Spectroscopy), MHz Original Text (NMR Spectroscopy) Location Reference
Chemical shifts
1H
chloroform-d1
1H-NMR (600 MHz, CDCI3) 5 4.01 (s, 4H), 3.75 - 3.66 (m, 8H), 1.46 (s, 18H).
Page/Page column 82
Current Patent Assignee: ASOCIACION CENTRO DE INVESTIGACION COOPERATIVA EN BIOCIENCIAS - WO2023/99741, 2023, A1



Chemical shifts, Spectrum
1H
chloroform-d1
400
supporting information
Bright, Sandra A.; Brinkø, Anne; Larsen, Maja Thim; Sinning, Steffen; Williams, D. Clive; Jensen, Henrik H.[Bioorganic and Medicinal Chemistry Letters, 2013, vol. 23, # 5, p. 1220 - 1224]


Chemical shifts, Spectrum
13C
chloroform-d1
100
supporting information
Bright, Sandra A.; Brinkø, Anne; Larsen, Maja Thim; Sinning, Steffen; Williams, D. Clive; Jensen, Henrik H.[Bioorganic and Medicinal Chemistry Letters, 2013, vol. 23, # 5, p. 1220 - 1224]


Chemical shifts
1H
CDCl3
Wittmann, Valentin; Takayama, Shuichi; Gong, Ke Wei; Weitz-Schmidt, Gabriele; Wong, Chi-Huey[Journal of Organic Chemistry, 1998, vol. 63, # 15, p. 5137 - 5143]


Chemical shifts
13C
CDCl3
Wittmann, Valentin; Takayama, Shuichi; Gong, Ke Wei; Weitz-Schmidt, Gabriele; Wong, Chi-Huey[Journal of Organic Chemistry, 1998, vol. 63, # 15, p. 5137 - 5143]



Mass Spectrometry - 3

Show/Hide columns
Description (Mass Spectrometry) Location Reference
electrospray ionisation (ESI), spectrum
Page/Page column 82
Current Patent Assignee: ASOCIACION CENTRO DE INVESTIGACION COOPERATIVA EN BIOCIENCIAS - WO2023/99741, 2023, A1


high resolution mass spectrometry (HRMS), electrospray ionisation (ESI), spectrum
Page/Page column 82
Current Patent Assignee: ASOCIACION CENTRO DE INVESTIGACION COOPERATIVA EN BIOCIENCIAS - WO2023/99741, 2023, A1


electrospray ionisation (ESI), high resolution mass spectrometry (HRMS), time-of-flight mass spectra (TOFMS), liquid chromatography mass spectrometry (LCMS), spectrum
supporting information
Bright, Sandra A.; Brinkø, Anne; Larsen, Maja Thim; Sinning, Steffen; Williams, D. Clive; Jensen, Henrik H.[Bioorganic and Medicinal Chemistry Letters, 2013, vol. 23, # 5, p. 1220 - 1224]

Chromatographic Data - 2

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Chromatographic data Original string Location Reference
HPLC (High performance liquid chromatography)
HPLC: tR = 18.42 min, gradient = 20-100percent solv. B over 30 min λmax = 200 nm.
Page/Page column 82
Current Patent Assignee: ASOCIACION CENTRO DE INVESTIGACION COOPERATIVA EN BIOCIENCIAS - WO2023/99741, 2023, A1


TLC (Thin layer chromatography)
supporting information
Bright, Sandra A.; Brinkø, Anne; Larsen, Maja Thim; Sinning, Steffen; Williams, D. Clive; Jensen, Henrik H.[Bioorganic and Medicinal Chemistry Letters, 2013, vol. 23, # 5, p. 1220 - 1224]

Crystal Property Description - 2

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Colour & Other Properties Location Reference
yellow
Page/Page column 153
Current Patent Assignee: MERCK PATENT GESELLSCHAFT MIT BESCHRANKTER HAFTUNG - WO2023/78813, 2023, A1


colourless
supporting information
Bright, Sandra A.; Brinkø, Anne; Larsen, Maja Thim; Sinning, Steffen; Williams, D. Clive; Jensen, Henrik H.[Bioorganic and Medicinal Chemistry Letters, 2013, vol. 23, # 5, p. 1220 - 1224]



и получение 3,6,9-trioxaundecane-1,11-dioic acid di-tert-butyl ester из bromoacetic acid tert-butyl ester и diethylene glycol


With sodium hydride In N,N-dimethyl-formamide 1.) 0 deg C, 30 min, 2.) room temp., 2 h;
48%
Wittmann, Valentin; Takayama, Shuichi; Gong, Ke Wei; Weitz-Schmidt, Gabriele; Wong, Chi-Huey
[Journal of Organic Chemistry, 1998, vol. 63, # 15, p. 5137 - 5143]


Stage #1: diethylene glycol With sodium hydride In N,N-dimethyl-formamide; mineral oil at 0℃; for 2h; Inert atmosphere;
Stage #2: bromoacetic acid tert-butyl ester In N,N-dimethyl-formamide; mineral oil at 0 - 20℃; Inert atmosphere;

Experimental Procedure
26%
Bright, Sandra A.; Brinkø, Anne; Larsen, Maja Thim; Sinning, Steffen; Williams, D. Clive; Jensen, Henrik H.
[Bioorganic and Medicinal Chemistry Letters, 2013, vol. 23, # 5, p. 1220 - 1224]


Stage #1: diethylene glycol With sodium hydride In N,N-dimethyl-formamide at 15℃;
Stage #2: bromoacetic acid tert-butyl ester In N,N-dimethyl-formamide at 0 - 15℃;

Experimental Procedure
39.7 %
Current Patent Assignee: MERCK PATENT GESELLSCHAFT MIT BESCHRANKTER HAFTUNG - WO2023/78813, 2023, A1
Location in patent: Page/Page column 153

[paramona]

Спасибо за помощь.