Hydrochloric Acid → 4-[(4E)-3-(4-Carboxybenzyl)-5-{2-[4-(4-fluorophenoxy)butoxy]phenyl}pent-4-en-1-yl]benzoic acid

HRID 1913803노트

반응식

HRID 1913803 반응식
C(C1C=[CH:42][C:6]([CH2:7][CH:8](/[CH:21]=[CH:22]/[C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][C:24]=2[O:29][CH2:30][CH2:31][CH2:32][CH2:33][O:34][C:35]2[CH:40]=[CH:39][C:38]([F:41])=[CH:37][CH:36]=2)[CH2:9][CH2:10][C:11]2[CH:20]=[CH:19][C:14]([C:15]([O:17]C)=[O:16])=[CH:13][CH:12]=2)=[CH:5][CH:4]=1)#N.[OH-:44].[K+].Cl.[CH2:47]([OH:50])[CH2:48][CH3:49]>O>[C:47]([C:48]1[CH:4]=[CH:5][C:6]([CH2:7][CH:8](/[CH:21]=[CH:22]/[C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][C:24]=2[O:29][CH2:30][CH2:31][CH2:32][CH2:33][O:34][C:35]2[CH:40]=[CH:39][C:38]([F:41])=[CH:37][CH:36]=2)[CH2:9][CH2:10][C:11]2[CH:12]=[CH:13][C:14]([C:15]([OH:17])=[O:16])=[CH:19][CH:20]=2)=[CH:42][CH:49]=1)([OH:50])=[O:44]

참가 물질

6

반응 조건

온도
110 °C

실험 절차

A solution of 460 mg (0.80 mmol) of methyl 4-[(4E)-3-(4-cyanobenzyl)-5-{2-[4-(4-fluorophenoxy)butoxy]phenyl}pent-4-en-1-yl]benzoate in 15 ml of 1-propanol and 2 ml of water is mixed with 1340 mg (23.89 mmol) of potassium hydroxide and stirred at 110° C. for 12 h. After cooling, the mixture is acidified with 1 M hydrochloric acid, and the crystals which have separated out are filtered off with suction, washed several times with water and dried. 325 mg (0.52 mmol, 65% of theory, purity 93%) of the title compound are obtained.

후처리

  1. temperatureAfter cooling
  2. customthe crystals which have separated out
  3. filtrationare filtered off with suction
  4. washwashed several times with water
  5. customdried

출처 및 근거

ORD 기록
ord-d59c9dd5f65f42839eda4a23b2d36661
출처 데이터셋
uspto-grants-2013_12
특허 번호
US08609727B2

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