Dichloromethane → 4-{[(4-Carboxybutyl)(2-{5-fluoro-2-[(4'-methyl-1,1'-biphenyl-4-yl)-methoxy]phenyl}ethyl)amino]methyl}benzoic acid

HRID 2110260ノート

反応式

HRID 2110260 の反応式
[F:1][C:2]1[CH:3]=[CH:4][C:5]([O:30][CH2:31][C:32]2[CH:37]=[CH:36][C:35]([C:38]3[CH:43]=[CH:42][C:41]([CH3:44])=[CH:40][CH:39]=3)=[CH:34][CH:33]=2)=[C:6]([CH2:8][CH2:9][N:10]([CH2:19][C:20]2[CH:29]=[CH:28][C:23]([C:24]([O:26]C)=[O:25])=[CH:22][CH:21]=2)[CH2:11][CH2:12][CH2:13][CH2:14][C:15]([O:17]C)=[O:16])[CH:7]=1.[OH-].[Na+].ClCCl>CO>[C:15]([CH2:14][CH2:13][CH2:12][CH2:11][N:10]([CH2:19][C:20]1[CH:29]=[CH:28][C:23]([C:24]([OH:26])=[O:25])=[CH:22][CH:21]=1)[CH2:9][CH2:8][C:6]1[CH:7]=[C:2]([F:1])[CH:3]=[CH:4][C:5]=1[O:30][CH2:31][C:32]1[CH:37]=[CH:36][C:35]([C:38]2[CH:43]=[CH:42][C:41]([CH3:44])=[CH:40][CH:39]=2)=[CH:34][CH:33]=1)([OH:17])=[O:16]

参加物

5

反応物 3

HCID 6344DichloromethaneHCID 14798Sodium HydroxideHCID 22015042Methyl 4-{[(2-{5-fluoro-2-[(4'-methyl-1,1'-biphenyl-4-yl)methoxy]phenyl}ethyl)(5-methoxy-5-oxopentyl)amino]methyl}benzoate

生成物 1

HCID 220150444-{[(4-Carboxybutyl)(2-{5-fluoro-2-[(4'-methyl-1,1'-biphenyl-4-yl)-methoxy]phenyl}ethyl)amino]methyl}benzoic acid

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

0.45 g (0.69 mmol) of methyl 4-{[(2-{5-fluoro-2-[(4′-methyl-1,1′-biphenyl-4-yl)methoxy]phenyl}ethyl)(5-methoxy-5-oxopentyl)amino]methyl}benzoate from Ex. 185 is dissolved in 8 ml of methanol. 0.5 ml of aqueous sodium hydroxide solution (45%) and 1.5 ml of dichloromethane are added, and the solution is stirred at RT for 8 hours. The reaction is extracted with diethyl ether, the aqueous phase is acidified using sulphuric acid and extracted with ethyl acetate and the extract is filtered through Extrelut and concentrated.

後処理

  1. extractionThe reaction is extracted with diethyl ether
  2. extractionextracted with ethyl acetate
  3. filtrationthe extract is filtered through Extrelut
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-b1650da1196743e4a4bf29a961fb8a3b
出典データセット
uspto-grants-2009_04
特許番号
US07517896B2

反応ノート

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