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

HRID 1913803ノート

反応式

HRID 1913803 の反応式
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]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 10311-PropanolHCID 14797Potassium HydroxideHCID 59180544Methyl 4-[(4E)-3-(4-cyanobenzyl)-5-{2-[4-(4-fluorophenoxy)butoxy]phenyl}pent-4-en-1-yl]benzoate

生成物 1

HCID 591804914-[(4E)-3-(4-Carboxybenzyl)-5-{2-[4-(4-fluorophenoxy)butoxy]phenyl}pent-4-en-1-yl]benzoic acid

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
110 °C

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-d59c9dd5f65f42839eda4a23b2d36661
出典データセット
uspto-grants-2013_12
特許番号
US08609727B2

反応ノート

読み込み中…