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Azide → Dimethyl 2-azidononanedioate

HRID 371378
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반응식

HRID 371378 반응식
[N-:1]=[N+:2]=[N-:3].Br[CH:5]([CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][C:16]([O:18][CH3:19])=[O:17])[C:6]([O:8][CH3:9])=[O:7]>C(#N)C>[N:1]([CH:15]([CH2:14][CH2:13][CH2:12][CH2:11][CH2:10][CH2:5][C:6]([O:8][CH3:9])=[O:7])[C:16]([O:18][CH3:19])=[O:17])=[N+:2]=[N-:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 33558AzideHCID 12760707Dimethyl 2-bromononanedioate

생성물 1

HCID 13251059Dimethyl 2-azidononanedioate수율 99.1%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

Soldium azide (4.87 g, 75 mmol) was added to a solution of dimethyl 2-bromoazelate (5.9 g, 20 mmol) prepared according to Auguston, M, et al; Acta Chim. Acad. Sci. Hung; 46:85 (1965) in acetonitrile, and the mixture was heated at reflux temperature for 4 h. The solvent was removed in vacuo, dichloromethane (80 ml) was added to the residue, and the mixture was washed with water. The organic phase was dried over sodium sulfate and the solvent was removed in vacuo to give the title compound as an oil (5.1 g, 98% yield).

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후처리

  1. customprepared
  2. temperatureat reflux temperature for 4 h
  3. customThe solvent was removed in vacuo, dichloromethane (80 ml)
  4. additionwas added to the residue
  5. washthe mixture was washed with water
  6. dry with materialThe organic phase was dried over sodium sulfate
  7. customthe solvent was removed in vacuo

출처 및 근거

ORD 기록
ord-4e8d13433170482a9249a7721e8ecc51
출처 데이터셋
uspto-grants-1985_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04532138

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