Hydrochloric Acid → (4-Phenylbutyl)phosphonic acid

HRID 651942

反応式

HRID 651942 の反応式
[C:1]1([CH2:7][CH2:8][CH2:9][CH2:10][P:11]([OH:13])[OH:12])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[OH-].[Na+].[Mn]([O-])(=O)(=O)=[O:17].[K+].Cl.S(=O)(O)[O-].[Na+]>CC(C)=O.O.C(OCC)(=O)C>[C:1]1([CH2:7][CH2:8][CH2:9][CH2:10][P:11](=[O:17])([OH:13])[OH:12])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

参加物

9

反応物 5

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 516875Potassium PermanganateHCID 132746654-Phenylbutylphosphonous acidHCID 23665763Sodium Bisulfite

生成物 1

HCID 13687984(4-Phenylbutyl)phosphonic acid

試薬・触媒・溶媒 3

HCID 180Acetone溶媒HCID 962Water溶媒3 回HCID 8857Ethyl Acetate溶媒

反応条件

温度
20 °C

実験手順

4-Phenylbutylphosphonous acid (47.19 gm, 0.238 mole) was dissolved in acetone (250 ml) and diluted with water (50 ml). Sodium hydroxide solution (9.5 gm, 0.238 mole) in water (50 ml) was added to it to get pH=7.0. The reaction mixture was cooled to 20° C. and potassium permanganate solution (22.5 gm, 0.142 mole) in water (250 ml) was added to it with stirring and maintaining the temperature around 20°-2 ° C. After the addition (15 minutes), the reaction mixture was stirred for 15 minutes at room temperature, acidified to pH 0 using concentrated HCl acid and saturated sodium bisulphite solution was added to it to get a white cloudy precipitate. Standard extractive workup using ethyl acetate followed by crystallization from ethyl acetate/hexane produced the title compound in 87% (44.16 gm) yield, m.p. 93° C.

後処理

  1. customto get pH=7.0
  2. temperaturemaintaining the temperature around 20°-2 ° C
  3. additionAfter the addition (15 minutes)
  4. stirringthe reaction mixture was stirred for 15 minutes at room temperature
  5. additionwas added to it
  6. customto get a white cloudy precipitate
  7. customfollowed by crystallization from ethyl acetate/hexane

出典と根拠

ORDレコード
ord-8bff35037c9c42e6be58d76192f8db73
出典データセット
uspto-grants-1987_06
特許番号
US04670193

関連ノート

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