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

HRID 1882309

反応式

HRID 1882309 の反応式
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

参加物

3

反応物 2

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

生成物 1

HCID 668114882-(4-Aminophenoxy)acetic acid hydrochloride収率 77.6%

反応条件

温度
10 °C

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-b5c2c6ad14dd433d84178d49c83c53c9
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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