Hydrochloric Acid → 4-(5-Chloro-2-methoxyphenyl)butanoic acid

HRID 2074012ノート

反応式

HRID 2074012 の反応式
O=[C:2]([C:8]1[CH:13]=[C:12]([Cl:14])[CH:11]=[CH:10][C:9]=1[O:15][CH3:16])[CH2:3][CH2:4][C:5]([OH:7])=[O:6].C1(C)C=CC=CC=1.Cl>O.[Zn]>[C:5]([CH2:4][CH2:3][CH2:2][C:8]1[CH:13]=[C:12]([Cl:14])[CH:11]=[CH:10][C:9]=1[O:15][CH3:16])([OH:7])=[O:6]

参加物

6

反応物 3

HCID 313Hydrochloric Acid2 回HCID 1140TolueneHCID 64970694-(5-Chloro-2-methoxy-phenyl)-4-oxo-butyric acid

生成物 1

HCID 124102564-(5-Chloro-2-methoxyphenyl)butanoic acid

試薬・触媒・溶媒 2

HCID 23994Zinc触媒HCID 962Water溶媒2 回

反応条件

温度
80 °C

実験手順

The acid compound of step 1 above is added to a stirring mixture of toluene (22 ml), conc HCl (41 ml), water (17 ml) and the recovered product of mossy zinc (22.2 g) and mercuric chloride (2.2 g) stirred in an aqueous HCl solution for about 10 minutes. The mixture is stirred under reflux for about 16 hours, diluted with water, extracted with ethyl acetate and the organic layer is dried filtered and evaporated. The residue is taken up in 10% aqueous NaOH, and dimethyl sulfate (about 25 ml) added to the mixture which is heated to 80° C. The mixture is stirred at a constant temperature for about 4 hours, cooled, acidified and the resulting precipitate is filtered dried and used in the next step.

後処理

  1. temperatureunder reflux for about 16 hours
  2. extractionextracted with ethyl acetate
  3. customthe organic layer is dried
  4. filtrationfiltered
  5. customevaporated
  6. additiondimethyl sulfate (about 25 ml) added to the mixture which
  7. stirringThe mixture is stirred at a constant temperature for about 4 hours
  8. temperaturecooled
  9. filtrationthe resulting precipitate is filtered
  10. customdried

出典と根拠

ORDレコード
ord-bf3bf98523004f5ab8749e5ca4dad799
出典データセット
uspto-grants-1990_04
特許番号
US04920219

反応ノート

読み込み中…