1,1',1''-(Chlorosilylidyne)tris(benzene) → Azidotriphenylsilane

HRID 1863200

반응식

HRID 1863200 반응식
[C:1]1([Si:7](Cl)([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[N-:21]=[N+:22]=[N-:23].[Li+]>O1CCCC1>[C:1]1([Si:7]([N:21]=[N+:22]=[N-:23])([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

참가 물질

4

반응물 2

HCID 64581,1',1''-(Chlorosilylidyne)tris(benzene)HCID 88163Lithium azide

생성물 1

HCID 79708Azidotriphenylsilane수율 86.3%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Following the method of Wiberg et al [Wiberg et al, Angew. Chem. Internat'l Ed.Engl., 1, 335 (1962)] in an inert atmosphere enclosure a solution of triphenylsilylchloride (73.9 g, 0.251 mol) in tetrahydrofuran (400 ml) was stirred with lithium azide (15.3 g, 0.312 mol) at room temperature over a period of 115 hr. After filtration, the solvent was removed in vacuo. The resulting white solid was boiled with heptane (350 ml), filtered hot and allowed to crystallize. Triphenylsilyl azide, 65.5 g (86.3% yield), mp 82°-84° C. was obtained. The melting point and infrared spectrum were identical with that of an authentic sample.

후처리

  1. filtrationAfter filtration
  2. customthe solvent was removed in vacuo
  3. filtrationfiltered hot
  4. customto crystallize

출처 및 근거

ORD 기록
ord-d8c4c5b25dce4a99a0091fa63cc0786a
출처 데이터셋
uspto-grants-1979_09
특허 번호
US04168287

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