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Water → 2-(1,4-Bis-(4-fluoro-phenyl)-1H-imidazol-2-yl)-1-(2-methyl-6,7-dihydro-4H-oxazolo[5,4-c]pyridin-5-yl)-ethanone

HRID 1019640
ノート
印刷プレビュー

反応式

HRID 1019640 の反応式
C(O[C:4](=[O:25])[CH2:5][C:6]1[N:7]([C:18]2[CH:23]=[CH:22][C:21]([F:24])=[CH:20][CH:19]=2)[CH:8]=[C:9]([C:11]2[CH:16]=[CH:15][C:14]([F:17])=[CH:13][CH:12]=2)[N:10]=1)C.Cl.[CH3:27][C:28]1[O:29][C:30]2[CH2:31][NH:32][CH2:33][CH2:34][C:35]=2[N:36]=1.CCN(C(C)C)C(C)C.O>CN1C(=O)CCC1>[F:24][C:21]1[CH:20]=[CH:19][C:18]([N:7]2[CH:8]=[C:9]([C:11]3[CH:12]=[CH:13][C:14]([F:17])=[CH:15][CH:16]=3)[N:10]=[C:6]2[CH2:5][C:4]([N:32]2[CH2:33][CH2:34][C:35]3[N:36]=[C:28]([CH3:27])[O:29][C:30]=3[CH2:31]2)=[O:25])=[CH:23][CH:22]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 81531DiisopropylethylamineHCID 86687938(1,4-bis-(4-fluoro-phenyl)-1H-imidazol-2-yl)-acetic acid ethyl esterHCID 866879402-Methyl-4,5,6,7-tetrahydrooxazolo[5,4-c]pyridine;hydrochloride

生成物 1

HCID 716042642-(1,4-Bis-(4-fluoro-phenyl)-1H-imidazol-2-yl)-1-(2-methyl-6,7-dihydro-4H-oxazolo[5,4-c]pyridin-5-yl)-ethanone収率 19.1%

試薬・触媒・溶媒 1

HCID 13387N-methyl-2-pyrrolidone溶媒

実験手順

70 mg (1,4-bis-(4-fluoro-phenyl)-1H-imidazol-2-yl)-acetic acid ethyl ester, 55 mg 2-methyl-4,5,6,7-tetrahydro-oxazolo[5,4-c]pyridine hydrochloride and 0.1 mL DIPEA in 2 mL NMP was stirred 50 min at 180° C. under microwave condition. The reaction was poured into water and extracted with EtOAC. The organic layer was dried with magnesium sulfate and evaporated the residue was purified by HPLC (Waters Symmetry 50×140 mm water+0,3% HCOOH/methanoll 10% until 90% in 14 min) to yield 17 mg desired product. Rt: 1.10 (method A), (M+H)+: 435

後処理

  1. extractionextracted with EtOAC
  2. dry with materialThe organic layer was dried with magnesium sulfate
  3. customevaporated the residue
  4. customwas purified by HPLC (Waters Symmetry 50×140 mm water+0,3% HCOOH/methanoll 10% until 90% in 14 min)

出典と根拠

ORDレコード
ord-2121e5c0a1d44fe89f5505877636c703
出典データセット
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08716277B2

反応ノート

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