Hydrochloric Acid → 3-Chloro-3-methyl-2-nitroso-1-butyl acetate

HRID 1076971

反応式

HRID 1076971 の反応式
[C:1]([O:4][CH2:5][CH:6]=[C:7]([CH3:9])[CH3:8])(=[O:3])[CH3:2].[N:10]([O:12]CCC(C)C)=O.[ClH:18]>C(O)(=O)C>[C:1]([O:4][CH2:5][CH:6]([N:10]=[O:12])[C:7]([Cl:18])([CH3:9])[CH3:8])(=[O:3])[CH3:2]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 8053Isoamyl NitriteHCID 14489Prenyl acetate

生成物 1

HCID 540488323-Chloro-3-methyl-2-nitroso-1-butyl acetate

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒2 回

実験手順

3,3-Dimethylallyl acetate (25 ml.), iso-amyl nitrite (45 ml.) and glacial acetic acid (65 ml.) were cooled in an ice-salt mixture. An ice-cold mixture of concentrated hydrochloric acid (20 ml.) and glacial acetic acid (20 ml.) was added gradually with stirring. The solution became green and towards the end of the addition a white solid precipitated. The solid was collected by filtration and dried (13 g.) Recrystallisation from CCl4 -- 40°/60° petrol gave the title compound as colourless needles (10 g.) m.p. 117°-119°.

後処理

  1. additionwas added gradually
  2. additionThe solution became green and towards the end of the addition a white solid
  3. customprecipitated
  4. filtrationThe solid was collected by filtration
  5. customdried
  6. custom(13 g.) Recrystallisation from CCl4

出典と根拠

ORDレコード
ord-61fa8655952e497390421b283761e33b
出典データセット
uspto-grants-1976_05
特許番号
US03959278

関連ノート

読み込み中…