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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0

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Azobisisobutyronitrile → 7-Bromomethyl-3,3-dimethyl-1-(2-trimethylsilanylethoxymethyl)-1,3-dihydroindol-2-one

HRID 1712519

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HRID 1712519 반응식

[CH3:1][C:2]1([CH3:21])[C:10]2[C:5](=[C:6]([CH3:11])[CH:7]=[CH:8][CH:9]=2)[N:4]([CH2:12][O:13][CH2:14][CH2:15][Si:16]([CH3:19])([CH3:18])[CH3:17])[C:3]1=[O:20].[Br:22]N1C(=O)CCC1=O.C(OOC(=O)C1C=CC=CC=1)(=O)C1C=CC=CC=1.N(C(C)(C)C#N)=NC(C)(C)C#N>C(Cl)(Cl)(Cl)Cl>[Br:22][CH2:11][C:6]1[CH:7]=[CH:8][CH:9]=[C:10]2[C:5]=1[N:4]([CH2:12][O:13][CH2:14][CH2:15][Si:16]([CH3:18])([CH3:17])[CH3:19])[C:3](=[O:20])[C:2]2([CH3:21])[CH3:1]

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참가 물질

6

반응물 4

HCID 6547Azobisisobutyronitrile

HCID 7187Benzoyl Peroxide

HCID 67184N-bromobutanimide

HCID 685015123,3,7-Trimethyl-1-(2-trimethylsilanylethoxymethyl)-1,3-dihydroindol-2-one

생성물 1

HCID 684977467-Bromomethyl-3,3-dimethyl-1-(2-trimethylsilanylethoxymethyl)-1,3-dihydroindol-2-one

시약·촉매·용매 1

HCID 5943

Carbon Tetrachloride

용매

실험 절차

The mixture of 3.10 g of 3,3,7-trimethyl-1-(2-trimethylsilanylethoxymethyl)-1,3-dihydroindol-2-one, 1.86 g of N-bromosuccinimide, 0.050 g of dibenzoyl peroxide and 0.033 g of 2,2′-azobis(2-methylpropionitrile) in 100 ml of carbon tetrachloride is kept at reflux with stirring over 2 hours. The reaction mixture is cooled and clarified by filtration, and the filtrate is concentrated by evaporation. The title compound is obtained as a beige solid from the residue by means of flash chromatography (SiO2 60F). Rf=0.42 (1:10 EtOAc-heptane); Rt=26.45 (II).

후처리

temperatureat reflux
temperatureThe reaction mixture is cooled
filtrationclarified by filtration
concentrationthe filtrate is concentrated by evaporation

출처 및 근거

ORD 기록: ord-2e35cdd313784f0ca8de196275a54a19
출처 데이터셋: uspto-grants-2010_09
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US07790715B2

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