Hydroxylamine HCl → HCID 189199、化合物

HRID 1683737ノート

反応式

HRID 1683737 の反応式
[CH:1](=[C:8]1[CH2:13][CH2:12][CH2:11][CH2:10][C:9]1=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[Cl-].[OH:16][NH3+:17]>C(O)C>[CH:1](=[C:8]1[CH2:13][CH2:12][CH2:11][CH2:10][C:9]1=[N:17][OH:16])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 21645Hydroxylamine HClHCID 989262-Benzylidenecyclohexanone

生成物 1

HCID 189199HCID 189199、化合物収率 97.8%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 2-benzylidenecyclohexanone (3.5 g, 18.8 mmol, J. Chem. Soc. 1949, 2957), hydroxylammonium chloride (3.9 g, 56 mmol) and ethanol (50 ml) was stirred at ambient temperature for 3 days. The solvent was evaporated in vacuo and the residue was dissolved in a mixture of ethyl acetate (200 ml) and water (50 ml). The phases were separated and the aqueous phase was extracted with ethyl acetate (50 ml). The combined organic extracts were washed with water and dried (MgSO4). The solvent was evaporated in vacuo to give 3.7 g of 2-benzylidenecyclohexanone oxime as a solid. M.p. 114°-115° C.

後処理

  1. customThe solvent was evaporated in vacuo
  2. dissolutionthe residue was dissolved in a mixture of ethyl acetate (200 ml) and water (50 ml)
  3. customThe phases were separated
  4. extractionthe aqueous phase was extracted with ethyl acetate (50 ml)
  5. washThe combined organic extracts were washed with water
  6. dry with materialdried (MgSO4)
  7. customThe solvent was evaporated in vacuo

出典と根拠

ORDレコード
ord-cf68406217e949d2857bab85922d0897
出典データセット
uspto-grants-1997_06
特許番号
US05639766

反応ノート

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