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Azobisisobutyronitrile → 1-[2-(Bromomethyl)-3,3-dimethylbut-1-en-1-yl]-2,4-dichlorobenzene

HRID 649518
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반응식

HRID 649518 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[CH:9]=[C:10]([CH3:15])[C:11]([CH3:14])([CH3:13])[CH3:12].[Br:16]N1C(=O)CCC1=O.CC(N=NC(C#N)(C)C)(C#N)C>ClC(Cl)C(Cl)Cl>[Br:16][CH2:15][C:10]([C:11]([CH3:14])([CH3:13])[CH3:12])=[CH:9][C:3]1[CH:4]=[CH:5][C:6]([Cl:8])=[CH:7][C:2]=1[Cl:1]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6547AzobisisobutyronitrileHCID 67184N-bromobutanimideHCID 53767202HCID 53767202, 화합물

생성물 1

HCID 545259841-[2-(Bromomethyl)-3,3-dimethylbut-1-en-1-yl]-2,4-dichlorobenzene수율 62.1%

시약·촉매·용매 1

HCID 65911,1,2,2-Tetrachloroethane용매

실험 절차

A mixture of 24.3 g (0.1 mol) of 1-(2,4-dichlorophenyl)-2,3,3-trimethylbut-1-ene, 17.8 g (0.1 mol) of N-bromosuccinimide and a spatula-tip of azodiisobutyrodinitrile in 100 ml of absolute 1,1,2,2-tetrachloroethane is boiled under reflux overnight. For working up, the mixture is concentrated in vacuo, the residue is taken up in carbon tetrachloride, the mixture is filtered and the filtrate is distilled. 20 g (62.1% of theory) of 2-bromomethyl-1-(2,4-dichlorophenyl)-3,3-dimethylbut-1-ene of boiling point 108° C. at 0.13 mbar are obtained. ##STR100##

후처리

  1. temperatureunder reflux overnight
  2. concentrationthe mixture is concentrated in vacuo
  3. filtrationthe mixture is filtered
  4. distillationthe filtrate is distilled

출처 및 근거

ORD 기록
ord-29adf584186d4acdb001ab9105ae1cfa
출처 데이터셋
uspto-grants-1988_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04740515

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