1,3,5-Tribromobenzene → Silane, 1,3,5-benzenetriyltris[triethoxy-

HRID 484190ノート

反応式

HRID 484190 の反応式
[CH2:1]([O:3][Si:4]([O:24][CH2:25][CH3:26])([O:21][CH2:22][CH3:23])[C:5]1[CH:10]=[CH:9][CH:8]=[C:7]([Si:11]([O:18][CH2:19][CH3:20])([O:15][CH2:16][CH3:17])[O:12][CH2:13][CH3:14])[CH:6]=1)[CH3:2].Br[C:28]1[CH:33]=C(Br)C=C(Br)C=1.[I-].[Cs+]>>[CH2:16]([O:15][Si:11]([O:12][CH2:13][CH3:14])([O:18][CH2:19][CH3:20])[C:7]1[CH:8]=[C:9]([Si:4]([O:24][CH2:33][CH3:28])([O:21][CH2:22][CH3:23])[O:3][CH2:1][CH3:2])[CH:10]=[C:5]([Si:4]([O:24][CH2:25][CH3:26])([O:21][CH2:22][CH3:23])[O:3][CH2:1][CH3:2])[CH:6]=1)[CH3:17]

参加物

4

反応物 3

HCID 122791,3,5-TribromobenzeneHCID 24601Cesium iodideHCID 116037721,3-Bis(triethoxysilyl)benzene

生成物 1

HCID 11713854Silane, 1,3,5-benzenetriyltris[triethoxy-

実験手順

The procedure used for the preparation of 1,3-di(triethoxysilyl)benzene was followed using 1,3,5-tribromobenzene (100.0 g, 0.318 mol) in place of 1,3-dibromobenzene. Two distillations gave a clear, colorless oil (0.1 mmHg, 196-198° C., 23.4 g, 13%). Anal. Calcd for C24H48O9Si3 : C, 51.0: H, 8.56. Found: C, 51.2; H, 8.53. IR (Neat, CsI, cm-1) : 2964 s, 2920 s, 2880 s, 2730 w, 1560 m, 1480 w, 1440 m, 1386 s, 1290 m, 1160 s, 1090 vs, 955 s, 825 s, 775 s, 710 m, 670 m, 487 s. 1H NMR (benzene -d6, 22° C., 300 MHz : δ 1.16 (t, J=7.1 Hz, 18 H, OCH2CH 3), 3.87 (q, J=7.1 Hz, 12 H, OCH2CH3, 8.55 (s, 1H, C6H4). 13C{1H} NMR (benzene-d6, 22° C., 75.5 MHz ): δ 18.43 (OCH2CH3), 58.92 (OCH2CH3), 130.83, 143.60 (C6H4).

後処理

  1. customTwo distillations gave a clear, colorless oil (0.1 mmHg, 196-198° C., 23.4 g, 13%)
  2. custom2964 s, 2920 s, 2880 s, 2730 w, 1560 m, 1480 w, 1440 m, 1386 s, 1290 m, 1160 s, 1090 vs, 955 s, 825 s, 775 s, 710 m, 670 m, 487 s
  3. custombenzene -d6, 22° C., 300 MHz

出典と根拠

ORDレコード
ord-b6f21b4eb82f4acf8a3c32a05281af82
出典データセット
uspto-grants-1993_07
特許番号
US05229481

反応ノート

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