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

HRID 484190노트

반응식

HRID 484190 반응식
[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]

참가 물질

4

반응물 3

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

생성물 1

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

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-b6f21b4eb82f4acf8a3c32a05281af82
출처 데이터셋
uspto-grants-1993_07
특허 번호
US05229481

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