Potassium Carbonate → Methyl 2-((S)-6-((R)-7-fluoro-4-(4-((2-methoxypyridin-4-yl)methoxy)-2,6-dimethylphenyl)-2,3-dihydro-1H-inden-1-yloxy)-2,3-dihydrobenzofuran-3-yl)acetate

HRID 237689ノート

反応式

HRID 237689 の反応式
[F:1][C:2]1[CH:3]=[CH:4][C:5]([C:26]2[C:31]([CH3:32])=[CH:30][C:29]([OH:33])=[CH:28][C:27]=2[CH3:34])=[C:6]2[C:10]=1[C@H:9]([O:11][C:12]1[CH:25]=[CH:24][C:15]3[C@H:16]([CH2:19][C:20]([O:22][CH3:23])=[O:21])[CH2:17][O:18][C:14]=3[CH:13]=1)[CH2:8][CH2:7]2.Cl.Cl[CH2:37][C:38]1[CH:43]=[CH:42][N:41]=[C:40]([O:44][CH3:45])[CH:39]=1.C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[F:1][C:2]1[CH:3]=[CH:4][C:5]([C:26]2[C:31]([CH3:32])=[CH:30][C:29]([O:33][CH2:37][C:38]3[CH:43]=[CH:42][N:41]=[C:40]([O:44][CH3:45])[CH:39]=3)=[CH:28][C:27]=2[CH3:34])=[C:6]2[C:10]=1[C@H:9]([O:11][C:12]1[CH:25]=[CH:24][C:15]3[C@H:16]([CH2:19][C:20]([O:22][CH3:23])=[O:21])[CH2:17][O:18][C:14]=3[CH:13]=1)[CH2:8][CH2:7]2

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 226250034-(Chloromethyl)-2-methoxypyridine hydrochlorideHCID 86697113Methyl 2-((S)-6-((R)-7-fluoro-4-(4-hydroxy-2,6-dimethylphenyl)-2,3-dihydro-1H-inden-1-yloxy)-2,3-dihydrobenzofuran-3-yl)acetate2 回

生成物 1

HCID 86697363Methyl 2-((S)-6-((R)-7-fluoro-4-(4-((2-methoxypyridin-4-yl)methoxy)-2,6-dimethylphenyl)-2,3-dihydro-1H-inden-1-yloxy)-2,3-dihydrobenzofuran-3-yl)acetate

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
60 °C

実験手順

Methyl 2-((S)-6-((R)-7-fluoro-4-(4-hydroxy-2,6-dimethylphenyl)-2,3-dihydro-1H-inden-1-yloxy)-2,3-dihydrobenzofuran-3-yl)acetate (Intermediate 28-29) (46.3 mg) and 4-(chloromethyl)-2-methoxypyridine hydrochloride (58.2 mg) were suspended in dimethylformamide (1.8 mL) and potassium carbonate (62 mg) was added. The reaction mixture was shaken for 24 h at 60° C. and than directly chromatographed by HPLC on reversed phase. The product fractions are collected and lyophilized to give the title compound. Yield: 42 mg; LC (method 23): tR=2.21 min; Mass spectrum (ESI+): m/z=584 [M+H]+.

後処理

  1. customthan directly chromatographed by HPLC on reversed phase
  2. customThe product fractions are collected

出典と根拠

ORDレコード
ord-509519b7e1f1438381d19806eb8ceac3
出典データセット
uspto-grants-2014_02
特許番号
US08642585B2

反応ノート

読み込み中…