Hydrochloric Acid → 4-{(4E)-3-(4-Carboxybenzyl)-5-[2-({4-[1,2,2,2-tetrafluoro-1-(trifluoromethyl)ethyl]benzyl}oxy)-phenyl]pent-4-en-1-yl}benzoic acid

HRID 1913801ノート

反応式

HRID 1913801 の反応式
C(C1C=[CH:47][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][C:31]2[CH:36]=[CH:35][C:34]([C:37]([F:46])([C:42]([F:45])([F:44])[F:43])[C:38]([F:41])([F:40])[F:39])=[CH:33][CH:32]=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-:49].[K+].Cl.[CH2:52]([OH:55])[CH2:53][CH3:54]>O>[C:52]([C:53]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][C:31]2[CH:36]=[CH:35][C:34]([C:37]([F:46])([C:38]([F:41])([F:39])[F:40])[C:42]([F:45])([F:43])[F:44])=[CH:33][CH:32]=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:47][CH:54]=1)([OH:49])=[O:55]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 10311-PropanolHCID 14797Potassium HydroxideHCID 59180492Methyl 4-{(4E)-3-(4-cyanobenzyl)-5-[2-({4-[1,2,2,2-tetrafluoro-1-(trifluoromethyl)ethyl]benzyl}-oxy)phenyl]pent-4-en-1-yl}benzoate

生成物 1

HCID 162255814-{(4E)-3-(4-Carboxybenzyl)-5-[2-({4-[1,2,2,2-tetrafluoro-1-(trifluoromethyl)ethyl]benzyl}oxy)-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 170 mg (0.25 mmol) of methyl 4-{(4E)-3-(4-cyanobenzyl)-5-[2-({4-[1,2,2,2-tetrafluoro-1-(trifluoromethyl)ethyl]benzyl}oxy)phenyl]pent-4-en-1-yl}benzoate in 3 ml of 1-propanol and 2 ml of water is mixed with 427 mg (7.6 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. 135 mg (0.2 mmol, 79% of theory) 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-6e89c895220549bcb7b3c0ef16d539a6
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…