Hydrochloric Acid → 2-(4-Aminophenoxy)acetic acid hydrochloride

HRID 1882309

반응식

HRID 1882309 반응식
C([O:3][C:4](=[O:17])[CH2:5][O:6][C:7]1[CH:12]=[CH:11][C:10]([NH:13]C(=O)C)=[CH:9][CH:8]=1)C.[ClH:18]>>[ClH:18].[NH2:13][C:10]1[CH:9]=[CH:8][C:7]([O:6][CH2:5][C:4]([OH:17])=[O:3])=[CH:12][CH:11]=1

참가 물질

3

반응물 2

HCID 313Hydrochloric AcidHCID 309738Ethyl 2-(4-acetamidophenoxy)acetate

생성물 1

HCID 668114882-(4-Aminophenoxy)acetic acid hydrochloride수율 77.6%

반응 조건

온도
10 °C

실험 절차

A mixture (4-acetylamino-phenoxy)-acetic acid ethyl ester 59 (375 grams, 1.582 mmol), in concentrated hydrochloric acid (9.36 liters) was refluxed for 12 hours. Excess concentrated hydrochloric acid was distilled off in vacuum and filtered hot. The mixture was cooled to 10° C., filtered and dried to give pure 60 (250 grams, 77.6%) as a wheat colored powder. The melting point was found to be 224-226° C. The structure was confirmed with NMR. IHNMR (D2O) δ 4.68 (s, 2H, OCH2), 3.65 (s, 3H, ester), 7.0 (d, 2H, Ar), 7.30 (d, 2H, Ar.

후처리

  1. distillationExcess concentrated hydrochloric acid was distilled off in vacuum
  2. filtrationfiltered hot
  3. filtrationfiltered
  4. customdried

출처 및 근거

ORD 기록
ord-b5c2c6ad14dd433d84178d49c83c53c9
출처 데이터셋
uspto-grants-2012_11
특허 번호
US08318973B2

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