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Dibutyltin oxide → 1-[1,2-diisopropoxyimino-2-(1H-tetrazol-5-yl)ethyl]-1H-1,2,4-triazole

HRID 339428
ノート
印刷プレビュー

反応式

HRID 339428 の反応式
[C:1]([C:3](=[N:15][O:16][CH:17]([CH3:19])[CH3:18])[C:4]([N:10]1[CH:14]=[N:13][CH:12]=[N:11]1)=[N:5][O:6][CH:7]([CH3:9])[CH3:8])#[N:2].C[Si]([N:24]=[N+:25]=[N-:26])(C)C.C([Sn](=O)CCCC)CCC>C1(C)C=CC=CC=1>[CH:7]([O:6][N:5]=[C:4]([N:10]1[CH:14]=[N:13][CH:12]=[N:11]1)[C:3](=[N:15][O:16][CH:17]([CH3:19])[CH3:18])[C:1]1[NH:26][N:25]=[N:24][N:2]=1)([CH3:9])[CH3:8]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 61221Dibutyltin oxideHCID 78378AzidotrimethylsilaneHCID 866815701-(2-cyano-1,2-diisopropoxyiminoethyl)-1H-1,2,4-triazole

生成物 1

HCID 1784601781-[1,2-diisopropoxyimino-2-(1H-tetrazol-5-yl)ethyl]-1H-1,2,4-triazole収率 49.6%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

To 5 ml of a toluene solution containing 0.40 g (1.51 mmol) of 1-(2-cyano-1,2-diisopropoxyiminoethyl)-1H-1,2,4-triazole were added 0.35 g (3.03 mmol) of trimethylsilylazide and 0.38 g (1.51 mmol) of di-n-butyltin oxide, followed by stirring for 3 hours under heating and refluxing. The reaction mixture was cooled to room temperature, followed by extraction with ethyl acetate. The extract solution was washed with an aqueous saturated sodium chloride solution and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (elutant:ethyl acetate/hexane=1/0). The crystal obtained was washed with isopropyl ether to obtain 0.23 g (yield: 47%) of a title compound.

後処理

  1. temperatureunder heating
  2. temperaturerefluxing
  3. extractionfollowed by extraction with ethyl acetate
  4. washThe extract solution was washed with an aqueous saturated sodium chloride solution
  5. dry with materialdried over anhydrous magnesium sulfate
  6. distillationThe solvent was distilled off under reduced pressure
  7. customThe residue was purified by silica gel column chromatography (elutant:ethyl acetate/hexane=1/0)
  8. customThe crystal obtained
  9. washwas washed with isopropyl ether

出典と根拠

ORDレコード
ord-fe00905b85794216a096c58262ac5b79
出典データセット
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08895035B2

反応ノート

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