Hydrochloric Acid → Methyl(4-aminophenoxy)acetate

HRID 1882310

反応式

HRID 1882310 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 (4-Amino-phenoxy)acetic acid HCl 60 (250 grams, 1.228 mol), in methanol (5 liters) was passed dry HCl gas at 10° C. for 1 hour and refluxed for 10 hours. Methanol (3.5 liters) was distilled and ice water (1 liter) was added and the pH was adjusted to 7.5 with K2CO3. Crude 61 was filtered, dried, and recrystallized from a mixture of Chloroform:Hexane (1:5) to give pure 61 (130 grams, 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
  5. additionice water (1 liter) was added
  6. filtrationCrude 61 was filtered
  7. customdried
  8. customrecrystallized from a mixture of Chloroform:Hexane (1:5)

出典と根拠

ORDレコード
ord-a035ee5898114d57826ef170fccf823c
出典データセット
uspto-grants-2012_11
特許番号
US08318973B2

関連ノート

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