Sodium Carbonate → Ammonia

HRID 2196189노트

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HRID 2196189 반응식
[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]

참가 물질

7

반응물 3

HCID 10340Sodium CarbonateHCID 14897375HCID 14897375, 화합물HCID 66931694HCID 66931694, 화합물

생성물 2

HCID 222AmmoniaHCID 56670260HCID 56670260, 화합물

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-4a099b9f3ae64f59934196a085765057
출처 데이터셋
uspto-grants-2012_12
특허 번호
US08338426B2

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