Ethanol → Tris(2,4-bis(N,N-bis(2-hydroxyethyl)sulfamoyl)phenyl)bismuthine

HRID 2839

Reaktionsgleichung

Reaktionsgleichung von HRID 2839
[Si]([O:8][CH2:9][CH2:10][N:11]([CH2:154][CH2:155][O:156][Si](C(C)(C)C)(C)C)[S:12]([C:15]1[CH:20]=[C:19]([S:21](=[O:44])(=[O:43])[N:22]([CH2:33][CH2:34][O:35][Si](C(C)(C)C)(C)C)[CH2:23][CH2:24][O:25][Si](C(C)(C)C)(C)C)[CH:18]=[CH:17][C:16]=1[Bi:45]([C:100]1[CH:105]=[CH:104][C:103]([S:106](=[O:129])(=[O:128])[N:107]([CH2:118][CH2:119][O:120][Si](C(C)(C)C)(C)C)[CH2:108][CH2:109][O:110][Si](C(C)(C)C)(C)C)=[CH:102][C:101]=1[S:130](=[O:153])(=[O:152])[N:131]([CH2:142][CH2:143][O:144][Si](C(C)(C)C)(C)C)[CH2:132][CH2:133][O:134][Si](C(C)(C)C)(C)C)[C:46]1[CH:51]=[CH:50][C:49]([S:52](=[O:75])(=[O:74])[N:53]([CH2:64][CH2:65][O:66][Si](C(C)(C)C)(C)C)[CH2:54][CH2:55][O:56][Si](C(C)(C)C)(C)C)=[CH:48][C:47]=1[S:76](=[O:99])(=[O:98])[N:77]([CH2:88][CH2:89][O:90][Si](C(C)(C)C)(C)C)[CH2:78][CH2:79][O:80][Si](C(C)(C)C)(C)C)(=[O:14])=[O:13])(C(C)(C)C)(C)C.C(O)C.O.C1(C)C=CC(S(O)(=O)=O)=CC=1>ClCCl>[OH:80][CH2:79][CH2:78][N:77]([CH2:88][CH2:89][OH:90])[S:76]([C:47]1[CH:48]=[C:49]([S:52](=[O:75])(=[O:74])[N:53]([CH2:64][CH2:65][OH:66])[CH2:54][CH2:55][OH:56])[CH:50]=[CH:51][C:46]=1[Bi:45]([C:100]1[CH:105]=[CH:104][C:103]([S:106](=[O:129])(=[O:128])[N:107]([CH2:118][CH2:119][OH:120])[CH2:108][CH2:109][OH:110])=[CH:102][C:101]=1[S:130](=[O:153])(=[O:152])[N:131]([CH2:142][CH2:143][OH:144])[CH2:132][CH2:133][OH:134])[C:16]1[CH:17]=[CH:18][C:19]([S:21](=[O:43])(=[O:44])[N:22]([CH2:33][CH2:34][OH:35])[CH2:23][CH2:24][OH:25])=[CH:20][C:15]=1[S:12](=[O:13])(=[O:14])[N:11]([CH2:10][CH2:9][OH:8])[CH2:154][CH2:155][OH:156])(=[O:98])=[O:99]

Komponenten

5

Edukt 3

HCID 702EthanolHCID 521998p-Toluenesulfonic acid monohydrateHCID 10606600tris(2,4-bis(N,N-bis(2-t-butyldimethylsilyloxyethyl)sulfamoyl)phenyl)bismuthine

Produkt 1

HCID 10844129Tris(2,4-bis(N,N-bis(2-hydroxyethyl)sulfamoyl)phenyl)bismuthineAusbeute 79,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Reaktionsbedingungen

Temperatur
50 °C

Versuchsvorschrift

13.59 g of the tris(2,4-bis(N,N-bis(2-t-butyldimethylsilyloxyethyl)sulfamoyl)phenyl)bismuthine preparation prepared in Example 5 was dissolved in a mixed solvent containing 13.6 ml of ethanol and 27 ml of dichloromethane, and 0.272 g of p-toluenesulfonic acid monohydrate was added thereto. The mixture was refluxed under heating at 50° C. for 6 hours, and then cooled to room temperature. The crystals were collected by filtration, washed with 29.5 ml of dichloromethane and dried. As a result, 5.54 g of the title compound was obtained as crystals with a melting point of 110°-113° C.

Aufarbeitung

  1. customprepared in Example 5
  2. dissolutionwas dissolved in a mixed solvent
  3. additionwas added
  4. temperatureThe mixture was refluxed
  5. temperaturecooled to room temperature
  6. filtrationThe crystals were collected by filtration
  7. washwashed with 29.5 ml of dichloromethane
  8. customdried

Quellen und Nachweise

ORD-Eintrag
ord-39d007a1ceb040768775ffb5002a1d9e
Quelldatensatz
uspto-grants-1998_03
Patentnummer
US05730953

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