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Azide → Dimethyl 2-azidononanedioate

HRID 371378
ノート
印刷プレビュー

反応式

HRID 371378 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 33558AzideHCID 12760707Dimethyl 2-bromononanedioate

生成物 1

HCID 13251059Dimethyl 2-azidononanedioate収率 99.1%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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).

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  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

出典と根拠

ORDレコード
ord-4e8d13433170482a9249a7721e8ecc51
出典データセット
uspto-grants-1985_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04532138

反応ノート

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