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Potassium Iodide → 1,4-dihydro-1-(2-iodoethyl)-4-methyl-5H-tetrazol-5-one

HRID 1863030
ノート
印刷プレビュー

反応式

HRID 1863030 の反応式
[I:1]C.Cl[CH2:4][CH2:5][N:6]1[C:10](=O)[NH:9][N:8]=[N:7]1.[C:12](=[O:15])([O-])[O-].[Na+].[Na+].[I-].[K+]>O.CC(C)CC(=O)C>[I:1][CH2:4][CH2:5][N:6]1[C:12](=[O:15])[N:9]([CH3:10])[N:8]=[N:7]1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 4875Potassium IodideHCID 6328Methyl iodideHCID 10340Sodium CarbonateHCID 1358293471-(2-chloroethyl)-1,4-dihydro-5H-tetrazol-5-one

生成物 1

HCID 136767191,4-dihydro-1-(2-iodoethyl)-4-methyl-5H-tetrazol-5-one収率 85%

試薬・触媒・溶媒 2

HCID 962Water
溶媒
2 回
HCID 7909Methyl Isobutyl Ketone溶媒

実験手順

A mixture of 49 parts of iodomethane, 10.5 parts of 1-(2-chloroethyl)-1,4-dihydro-5H-tetrazol-5-one, 15 parts of sodium carbonate, 0.2 parts of potassium iodide and 240 parts of 4-methyl-2-pentanone is stirred and refluxed overnight with water-separator. The reaction mixture is cooled, 100 parts of water are added and the layers are separated. The aqueous phase is extracted with dichloromethane. The combined organic phases are dried, filtered and evaporated. The residue is purified by column-chromatography over silica gel using trichloromethane as eluent. The pure fractions are collected and the eluent is evaporated, yielding 15 parts (85%) of 1,4-dihydro-1-(2-iodoethyl)-4-methyl-5H-tetrazol-5-one as a residue.

後処理

  1. temperatureThe reaction mixture is cooled
  2. customthe layers are separated
  3. extractionThe aqueous phase is extracted with dichloromethane
  4. customThe combined organic phases are dried
  5. filtrationfiltered
  6. customevaporated
  7. customThe residue is purified by column-chromatography over silica gel
  8. customThe pure fractions are collected
  9. customthe eluent is evaporated

出典と根拠

ORDレコード
ord-ca68393763014a85a584fef82393eec1
出典データセット
uspto-grants-1979_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04167574

反応ノート

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