Ethanol → HCID 86686776、化合物

HRID 1403142

反応式

HRID 1403142 の反応式
[F:1][CH:2]([F:32])[C:3]1[N:7]([C:8]2[CH:13]=[C:12]([N:14]3[CH2:19][CH2:18][O:17][CH2:16][CH2:15]3)[N:11]=[C:10]([NH:20][CH2:21][CH:22]3[CH2:27][CH2:26][NH:25][CH2:24][CH2:23]3)[N:9]=2)[C:6]2[CH:28]=[CH:29][CH:30]=[CH:31][C:5]=2[N:4]=1.C(O)C.[F:36][CH2:37][CH:38]1[CH2:40][O:39]1.C(N(CC)C(C)C)(C)C>O>[F:32][CH:2]([F:1])[C:3]1[N:7]([C:8]2[CH:13]=[C:12]([N:14]3[CH2:19][CH2:18][O:17][CH2:16][CH2:15]3)[N:11]=[C:10]([NH:20][CH2:21][CH:22]3[CH2:23][CH2:24][N:25]([CH2:40][CH:38]([OH:39])[CH2:37][F:36])[CH2:26][CH2:27]3)[N:9]=2)[C:6]2[CH:28]=[CH:29][CH:30]=[CH:31][C:5]=2[N:4]=1

参加物

6

反応物 4

HCID 702EthanolHCID 104181,2-Epoxy-3-fluoropropaneHCID 81531DiisopropylethylamineHCID 86686777HCID 86686777、化合物

生成物 1

HCID 86686776HCID 86686776、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
120 °C

実験手順

To a mixture of 4-[2-(difluoromethyl)-1H-benzimidazol-1-yl]-6-morpholin-4-yl-N-(piperidin-4-ylmethyl)pyrimidin-2-amine (100 mg) and ethanol (2 mL) were added 2-(fluoromethyl)oxirane (19 μL) and N,N-diisopropyl ethylamine (79 μL), and the mixture was stirred in a microwave reactor at 120° C. for 1 hour. To the reaction mixture was added water, followed by extraction with ethyl acetate. The organic layer was washed with saturated brine and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure and then the residue was purified by amino silica gel column chromatography (ethyl acetate:hexane) to obtain 1-{4-[({4-[2-(difluoromethyl)-1H-benzimidazol-1-yl]-6-(morpholin-4-yl)pyrimidin-2-yl}amino)methyl]piperidin-1-yl}-3-fluoropropan-2-ol (81 mg) as a white powder.

後処理

  1. extractionfollowed by extraction with ethyl acetate
  2. washThe organic layer was washed with saturated brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customThe solvent was evaporated under reduced pressure
  5. customthe residue was purified by amino silica gel column chromatography (ethyl acetate:hexane)

出典と根拠

ORDレコード
ord-38e3e188e5524b7691b98d0105a36a12
出典データセット
uspto-grants-2014_12
特許番号
US08912180B2

関連ノート

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