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Acetonitrile → Pentanenitrile, 4,4-dimethyl-3-oxo-

HRID 128431
ノート
印刷プレビュー

反応式

HRID 128431 の反応式
[H-].[Na+].[C:3]([O:9]C)(=O)[C:4]([CH3:7])([CH3:6])[CH3:5].[C:11](#[N:13])[CH3:12]>O1CCCC1>[C:3]([CH2:12][C:11]#[N:13])(=[O:9])[C:4]([CH3:7])([CH3:6])[CH3:5]
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 6342AcetonitrileHCID 24758Sodium hydrideHCID 69027Methyl pivalate

生成物 1

HCID 108871Pentanenitrile, 4,4-dimethyl-3-oxo-

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

In a 1 l. flask under an atmosphere of dry nitrogen there was placed 26.4 g. of a 50% oil dispersion of sodium hydride together with 240 ml. of dry tetrahydrofuran. While this mixture was refluxed there was added thereto dropwise over a period of about 1 hour a mixture of 40.6 g. of methyl pivalate and 22.6 g. of acetonitrile in 40 ml. of dry tetrahydrofuran. When addition was complete, the mixture was refluxed overnight. The reaction mixture was worked up by evaporating part of the tetrahydrofuran in vacuo and dissolving the remaining solution in about 300 ml. of water. This aqueous mixture was acidified to about pH 4 using concentrated aqueous hydrochloric acid. The remainder of the tetrahydrofuran was then removed using a rotovapor. The solid which was formed was filtered and slurried with 150 ml. of hexane to remove mineral oil. The crystals were filtered and dried. The crystals had a melting point of about 57°-59° C. and were identified as pivalyl acetonitrile. Yield: 36.3 g. (83%).

後処理

  1. customflask under an atmosphere of dry nitrogen there was placed
  2. temperatureWhile this mixture was refluxed there
  3. additionwas added
  4. additiondropwise over a period of about 1 hour a mixture of 40.6 g
  5. additionWhen addition
  6. temperaturethe mixture was refluxed overnight
  7. customby evaporating part of the tetrahydrofuran in vacuo
  8. dissolutiondissolving the remaining solution in about 300 ml
  9. customThe remainder of the tetrahydrofuran was then removed
  10. customThe solid which was formed
  11. filtrationwas filtered
  12. customof hexane to remove mineral oil
  13. filtrationThe crystals were filtered
  14. customdried

出典と根拠

ORDレコード
ord-355fc2bf84d64590b798bae7814bd719
出典データセット
uspto-grants-1981_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04259501

反応ノート

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