Sodium Carbonate → Ammonia

HRID 2196189ノート

反応式

HRID 2196189 の反応式
[F:1][C:2]1[CH:3]=[C:4]([NH:14][C:15]([C:17]2[C:18]([C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=3)=[CH:19][CH:20]=[CH:21][CH:22]=2)=[O:16])[CH:5]=[CH:6][C:7]=1[N:8]1[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]1.Br[CH:30]([C:38]1[CH:43]=[CH:42][CH:41]=[CH:40][CH:39]=1)[C:31]([N:33]([CH2:36][CH3:37])[CH2:34][CH3:35])=[O:32].C([O-])([O-])=O.[Na+].[Na+]>CN(C=O)C.CCOC(C)=O>[NH3:8].[CH2:36]([N:33]([CH2:34][CH3:35])[C:31]([CH:30]([C:38]1[CH:43]=[CH:42][CH:41]=[CH:40][CH:39]=1)[N:11]1[CH2:12][CH2:13][N:8]([C:7]2[CH:6]=[CH:5][C:4]([NH:14][C:15]([C:17]3[C:18]([C:23]4[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=4)=[CH:19][CH:20]=[CH:21][CH:22]=3)=[O:16])=[CH:3][C:2]=2[F:1])[CH2:9][CH2:10]1)=[O:32])[CH3:37]

参加物

7

反応物 3

HCID 10340Sodium CarbonateHCID 14897375HCID 14897375、化合物HCID 66931694HCID 66931694、化合物

生成物 2

HCID 222AmmoniaHCID 56670260HCID 56670260、化合物

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

A solution of biphenyl-2-carboxylic acid (3-fluoro-4-piperazin-1-yl-phenyl)-amide (0.030 g, 0.08 mmol), 2-bromo-N,N-diethyl-2-phenyl-acetamide (0.025 g, 0.09 mmol), and Na2CO3 (0.013 g, 0.1 mmol) in DMF (2 mL) was stirred at room temperature. After 18 h, the reaction mixture was diluted with EtOAc (25 mL) and washed with H2O (3×15 mL). The organic layers were combined, dried (Na2SO4), and concentrated. Chromatography of the resulting residue (SiO2: 2 M NH3 in MeOH/CH2Cl2) yielded the title compound.

後処理

  1. washwashed with H2O (3×15 mL)
  2. dry with materialdried (Na2SO4)
  3. concentrationconcentrated

出典と根拠

ORDレコード
ord-4a099b9f3ae64f59934196a085765057
出典データセット
uspto-grants-2012_12
特許番号
US08338426B2

反応ノート

読み込み中…