Methanesulfonic Acid → 3-(2-fluoro-4-{[4-({5-(2-phenylethyl)-3-[4-(trifluoromethyl)phenyl]-1H-pyrazol-1-yl}methyl)benzyl]amino}phenyl)propanoic acid methanesulfonate

HRID 508055ノート

反応式

HRID 508055 の反応式
[F:1][C:2]1[CH:7]=[C:6]([NH:8][CH2:9][C:10]2[CH:15]=[CH:14][C:13]([CH2:16][N:17]3[C:21]([CH2:22][CH2:23][C:24]4[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=4)=[CH:20][C:19]([C:30]4[CH:35]=[CH:34][C:33]([C:36]([F:39])([F:38])[F:37])=[CH:32][CH:31]=4)=[N:18]3)=[CH:12][CH:11]=2)[CH:5]=[CH:4][C:3]=1[CH2:40][CH2:41][C:42]([OH:44])=[O:43].[CH3:45][S:46]([OH:49])(=[O:48])=[O:47]>C(OCC)(=O)C>[CH3:45][S:46]([OH:49])(=[O:48])=[O:47].[F:1][C:2]1[CH:7]=[C:6]([NH:8][CH2:9][C:10]2[CH:15]=[CH:14][C:13]([CH2:16][N:17]3[C:21]([CH2:22][CH2:23][C:24]4[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=4)=[CH:20][C:19]([C:30]4[CH:31]=[CH:32][C:33]([C:36]([F:38])([F:37])[F:39])=[CH:34][CH:35]=4)=[N:18]3)=[CH:12][CH:11]=2)[CH:5]=[CH:4][C:3]=1[CH2:40][CH2:41][C:42]([OH:44])=[O:43]

参加物

4

反応物 2

HCID 6395Methanesulfonic AcidHCID 231574013-(2-fluoro-4-{[4-({5-(2-phenylethyl)-3-[4-(trifluoromethyl)phenyl]-1H-pyrazol-1-yl}methyl)benzyl]amino}phenyl)propanoic acid

生成物 1

HCID 866243773-(2-fluoro-4-{[4-({5-(2-phenylethyl)-3-[4-(trifluoromethyl)phenyl]-1H-pyrazol-1-yl}methyl)benzyl]amino}phenyl)propanoic acid methanesulfonate収率 60.1%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of 3-(2-fluoro-4-{[4-({5-(2-phenylethyl)-3-[4-(trifluoromethyl)phenyl]-1H-pyrazol-1-yl}methyl)benzyl]amino}phenyl)propanoic acid (500 mg, 0.83 mmol) in ethyl acetate (20 mL) was added methanesulfonic acid (95 mg, 1.0 mmol) at room temperature, and the mixture was stirred for 1 hr. The reaction mixture was concentrated, isopropyl ether was added and the precipitated crystals were collected by filtration, washed with isopropyl ether and dried to give the title compound as colorless crystals (348 mg, yield 60%).

後処理

  1. concentrationThe reaction mixture was concentrated
  2. additionisopropyl ether was added
  3. filtrationthe precipitated crystals were collected by filtration
  4. washwashed with isopropyl ether
  5. customdried

出典と根拠

ORDレコード
ord-34d00a36266347b39c113dfdcddfa1ea
出典データセット
uspto-grants-2010_08
特許番号
US07786165B2

反応ノート

読み込み中…