Triethylamine → 2,4,8,10-Tetra-t-butyl-6-phenyl-12H-dibenzo[d,g][1,3,2]dioxasilocin

HRID 1380706

반응식

HRID 1380706 반응식
Cl[SiH:2](Cl)[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[CH2:10]([C:26]1[CH:31]=[C:30]([C:32]([CH3:35])([CH3:34])[CH3:33])[CH:29]=[C:28]([C:36]([CH3:39])([CH3:38])[CH3:37])[C:27]=1[OH:40])[C:11]1[CH:16]=[C:15]([C:17]([CH3:20])([CH3:19])[CH3:18])[CH:14]=[C:13]([C:21]([CH3:24])([CH3:23])[CH3:22])[C:12]=1[OH:25].C(N(CC)CC)C>>[C:32]([C:30]1[CH:29]=[C:28]([C:36]([CH3:39])([CH3:38])[CH3:37])[C:27]2[O:40][SiH:2]([C:3]3[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=3)[O:25][C:12]3[C:13]([C:21]([CH3:23])([CH3:22])[CH3:24])=[CH:14][C:15]([C:17]([CH3:20])([CH3:19])[CH3:18])=[CH:16][C:11]=3[CH2:10][C:26]=2[CH:31]=1)([CH3:35])([CH3:34])[CH3:33]

참가 물질

4

반응물 3

HCID 8471TriethylamineHCID 74207Dichloro(phenyl)silaneHCID 843912,2'-Methylenebis(4,6-di-tert-butylphenol)

생성물 1

HCID 1317141472,4,8,10-Tetra-t-butyl-6-phenyl-12H-dibenzo[d,g][1,3,2]dioxasilocin수율 64.3%

실험 절차

Utilizing the procedure of Example 1, this compound is prepared from 17.7 grams (0.1 mole) of dichlorophenylsilane, 42.5 grams (0.1 mole) of 2,2'-methylenebis(4,6-di-t-butylphenol) and 20.2 grams (0.20 mole) of triethylamine. Recrystallization twice from acetonitrile-toluene yields 34.0 grams (64% yield) of product as an off white powder, mp 153°-156° C.; IR: 2200 cm-1SiH.

후처리

  1. customRecrystallization twice from acetonitrile-toluene

출처 및 근거

ORD 기록
ord-5db59391d9ff4c1d9370aab3ee4b2a84
출처 데이터셋
uspto-grants-1986_04
특허 번호
US04582870

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