Hydrochloric Acid → Methyl(4-aminophenoxy)acetate

HRID 638707

反応式

HRID 638707 の反応式
Cl.[NH2:2][C:3]1[CH:13]=[CH:12][C:6]([O:7][CH2:8][C:9]([OH:11])=[O:10])=[CH:5][CH:4]=1.Cl.[CH3:15]O>>[CH3:15][O:10][C:9](=[O:11])[CH2:8][O:7][C:6]1[CH:5]=[CH:4][C:3]([NH2:2])=[CH:13][CH:12]=1

参加物

4

反応物 3

HCID 313Hydrochloric AcidHCID 887MethanolHCID 668114882-(4-Aminophenoxy)acetic acid hydrochloride

生成物 1

HCID 6422115Methyl(4-aminophenoxy)acetate収率 58.5%

実験手順

To a mixture of (4-Aminophenoxy)acetic acid HCl 14 (250 g, 1.228 mol), in methanol (5 L) was passed dry HCl gas at 10° C. for 1 hour and refluxed for 10 hours. Methanol (3.5 liters) was distilled off, ice water (1 liter) was added and the pH was adjusted to 7.5 with K2CO3. Crude 15 was filtered, dried and recrystallised from a mixture of chloroform:hexane (1:5) to give pure 15 (130 g, 58.5%) as a light brown powder. The melting point was found to be 65-66.8° C.

後処理

  1. customat 10° C.
  2. customfor 1 hour
  3. temperaturerefluxed for 10 hours
  4. distillationMethanol (3.5 liters) was distilled off
  5. additionice water (1 liter) was added
  6. filtrationCrude 15 was filtered
  7. customdried
  8. customrecrystallised from a mixture of chloroform:hexane (1:5)

出典と根拠

ORDレコード
ord-23114a76f8bc498c981544969feddb83
出典データセット
uspto-grants-2010_04
特許番号
US07691364B2

関連ノート

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