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Sodium Iodide → 3-[(3-{4-[5-Acetyl-1-(3-fluoropropyl)-1H-pyrrol-3-yl]-2-amino-1-methyl-5-oxo-4,5-dihydro-1H-imidazol-4-yl}phenoxy)methyl]benzamide

HRID 2220475
ノート
印刷プレビュー

反応式

HRID 2220475 の反応式
[C:1]([C:4]1[N:8]([CH2:9][CH2:10][CH2:11][F:12])[CH:7]=[C:6]([C:13]2([C:21]3[CH:26]=[CH:25][CH:24]=[C:23]([OH:27])[CH:22]=3)[N:17]=[C:16]([NH2:18])[N:15]([CH3:19])[C:14]2=[O:20])[CH:5]=1)(=[O:3])[CH3:2].Cl[CH2:29][C:30]1[CH:31]=[C:32]([CH:36]=[CH:37][CH:38]=1)[C:33]([NH2:35])=[O:34].[I-].[Na+].C(=O)([O-])[O-].[Cs+].[Cs+]>CN(C)C=O.C(OCC)(=O)C>[C:1]([C:4]1[N:8]([CH2:9][CH2:10][CH2:11][F:12])[CH:7]=[C:6]([C:13]2([C:21]3[CH:22]=[C:23]([CH:24]=[CH:25][CH:26]=3)[O:27][CH2:29][C:30]3[CH:31]=[C:32]([CH:36]=[CH:37][CH:38]=3)[C:33]([NH2:35])=[O:34])[C:14](=[O:20])[N:15]([CH3:19])[C:16]([NH2:18])=[N:17]2)[CH:5]=1)(=[O:3])[CH3:2]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 5238Sodium IodideHCID 10796Cesium carbonateHCID 7371453-Chloromethyl-benzamideHCID 597726545-[5-acetyl-1-(3-fluoropropyl)-1H-pyrrol-3-yl]-2-amino-5-(3-hydroxyphenyl)-3-methyl-3,5-dihydro-4H-imidazol-4-one

生成物 1

HCID 597727593-[(3-{4-[5-Acetyl-1-(3-fluoropropyl)-1H-pyrrol-3-yl]-2-amino-1-methyl-5-oxo-4,5-dihydro-1H-imidazol-4-yl}phenoxy)methyl]benzamide

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
45 °C

実験手順

A mixture of 5-[5-acetyl-1-(3-fluoropropyl)-1H-pyrrol-3-yl]-2-amino-5-(3-hydroxyphenyl)-3-methyl-3,5-dihydro-4H-imidazol-4-one, 3-(chloromethyl)benzamide, sodium iodide, and cesium carbonate in dimethylformamide was heated to 45° C. for 16 hours. The cooled reaction mixture was poured into ethyl acetate and washed with water. The organic phase was dried over sodium sulfate and evaporated. The resultant residue was purified by HPLC using a CN bonded phase preparative column and by precipitation from hexane to give the title product as a white solid, identified by NMR and mass spectral analyses.

後処理

  1. customThe cooled reaction mixture
  2. washwashed with water
  3. dry with materialThe organic phase was dried over sodium sulfate
  4. customevaporated
  5. customThe resultant residue was purified by HPLC
  6. customby precipitation from hexane

出典と根拠

ORDレコード
ord-197137909d54496ca9b52a5371aaed4a
出典データセット
uspto-grants-2008_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07417047B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート