Water → 2-[4-(2-Hydroxyiminocyclohexan-1-ylmethyl)phenyl]propionic Acid

HRID 971868ノート

反応式

HRID 971868 の反応式
O=[C:2]1[CH2:7][CH2:6][CH2:5][CH2:4][CH:3]1[CH2:8][C:9]1[CH:14]=[CH:13][C:12]([CH:15]([CH3:19])[C:16]([OH:18])=[O:17])=[CH:11][CH:10]=1.Cl.[NH2:21][OH:22].O.O.O.C([O-])(=O)C.[Na+].O>C(O)C>[OH:22][N:21]=[C:2]1[CH2:7][CH2:6][CH2:5][CH2:4][CH:3]1[CH2:8][C:9]1[CH:14]=[CH:13][C:12]([CH:15]([CH3:19])[C:16]([OH:18])=[O:17])=[CH:11][CH:10]=1

参加物

6

反応物 4

HCID 962WaterHCID 443297Hydroxyamine hydrochlorideHCID 133914932-(4-((2-Oxocyclohexyl)methyl)phenyl)propanoic acidHCID 23665404Sodium Acetate Trihydrate

生成物 1

HCID 737697732-[4-(2-Hydroxyiminocyclohexan-1-ylmethyl)phenyl]propionic Acid収率 107.1%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of 1.3 g of 2-[4-(2-oxocyclohexan-1-ylmethyl)phenyl]propionic acid, 0.33 g of hydroxylamine hydrochloride and 1.6 g of sodium acetate trihydrate in 85% ethanol was heated with stirring at 70°-75° C. for 2 hours, and the mixture was poured into 100 ml of water and extracted with ether. The extract was washed with water, dried over anhydrous sodium sulfate, and the solvent removed by distillation to give 1.4 g of the desired compound, which by recrystallization from a mixture of ethyl acetate and n-hexane afforded colorless prisms, m.p. 143°-150.5° C.

後処理

  1. extractionextracted with ether
  2. washThe extract was washed with water
  3. dry with materialdried over anhydrous sodium sulfate
  4. customthe solvent removed by distillation

出典と根拠

ORDレコード
ord-9ea146a4363d467f8afc88b4fb100801
出典データセット
uspto-grants-1979_07
特許番号
US04161538

反応ノート

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