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Ethyl Acetate → Acetic Acid 2-{4-chloro-6-[2-(3-fluoro-pyridin-2-yl)-imidazol-1-ylmethyl]-pyrimidin-5-yl}-ethyl ester

HRID 916658
ノート
印刷プレビュー

反応式

HRID 916658 の反応式
Br[CH2:2][C:3]1[C:8]([CH2:9][CH2:10][O:11][C:12](=[O:14])[CH3:13])=[C:7]([Cl:15])[N:6]=[CH:5][N:4]=1.[F:16][C:17]1[C:18]([C:23]2[NH:24][CH:25]=[CH:26][N:27]=2)=[N:19][CH:20]=[CH:21][CH:22]=1.C([O-])([O-])=O.[K+].[K+].CCOC(C)=O>CN(C=O)C.O>[Cl:15][C:7]1[C:8]([CH2:9][CH2:10][O:11][C:12](=[O:14])[CH3:13])=[C:3]([CH2:2][N:24]2[CH:25]=[CH:26][N:27]=[C:23]2[C:18]2[C:17]([F:16])=[CH:22][CH:21]=[CH:20][N:19]=2)[N:4]=[CH:5][N:6]=1
参加物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 8857Ethyl AcetateHCID 11430Potassium CarbonateHCID 223131643-Fluoro-2-(1H-imidazol-2-yl)pyridineHCID 57503307Acetic Acid 2-(4-bromomethyl-6-chloro-pyrimidin-5-yl)-ethyl ester

生成物 1

HCID 57503309Acetic Acid 2-{4-chloro-6-[2-(3-fluoro-pyridin-2-yl)-imidazol-1-ylmethyl]-pyrimidin-5-yl}-ethyl ester

試薬・触媒・溶媒 2

HCID 962
Water
溶媒
HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 162 (8.4 mmol), 3-fluoro-2-(1H-imidazol-2-yl)-pyridine (described above) (1.38 g, 8.4 mmol) and K2CO3 (1.17 g, 8.4 mmol) in DMF (6 ml) is stirred at room temperature overnight. To the mixture are added EtOAc (20 ml) and water (10 ml). The organic layer is separated and the aqueous layer is extracted with EtOAc (3×10 ml). The combined extracts are washed with brine (10 ml), dried (Na2SO4) and solvent evaporated. PTLC separation of the residue (5% MeOH in CH2Cl2) gives the product (163) as a white solid.

後処理

  1. customThe organic layer is separated
  2. extractionthe aqueous layer is extracted with EtOAc (3×10 ml)
  3. washThe combined extracts are washed with brine (10 ml)
  4. dry with materialdried (Na2SO4) and solvent
  5. customevaporated
  6. customPTLC separation of the residue (5% MeOH in CH2Cl2)

出典と根拠

ORDレコード
ord-3ae0893890ae449489ee12669ddcd425
出典データセット
uspto-grants-2007_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07271170B2

反応ノート

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