Hydrochloric Acid → Methyl(4-aminophenoxy)acetate

HRID 638707

반응식

HRID 638707 반응식
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

참가 물질

4

반응물 3

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

생성물 1

HCID 6422115Methyl(4-aminophenoxy)acetate수율 58.5%

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-23114a76f8bc498c981544969feddb83
출처 데이터셋
uspto-grants-2010_04
특허 번호
US07691364B2

연결된 노트

불러오는 중…