Sodium Carbonate → HCID 86628364, 화합물

HRID 2233195노트

반응식

HRID 2233195 반응식
CC1C=CC(S(O[CH2:12][C:13]2([OH:27])[C:23]3[C:24]4[N:15]([C:16](=[O:26])[CH:17]=[N:18][C:19]=4[CH:20]=[CH:21][C:22]=3[F:25])[CH2:14]2)(=O)=O)=CC=1.[O:28]1[C:37]2[CH:36]=[C:35]([CH2:38][N:39]([CH:47]3[CH2:52][CH2:51][NH:50][CH2:49][CH2:48]3)[C:40](=[O:46])[O:41][C:42]([CH3:45])([CH3:44])[CH3:43])[N:34]=[CH:33][C:32]=2[O:31][CH2:30][CH2:29]1.C(=O)([O-])[O-].[Na+].[Na+]>C(O)C>[O:28]1[C:37]2[CH:36]=[C:35]([CH2:38][N:39]([CH:47]3[CH2:52][CH2:51][N:50]([CH2:12][C:13]4([OH:27])[C:23]5[C:24]6[N:15]([C:16](=[O:26])[CH:17]=[N:18][C:19]=6[CH:20]=[CH:21][C:22]=5[F:25])[CH2:14]4)[CH2:49][CH2:48]3)[C:40](=[O:46])[O:41][C:42]([CH3:45])([CH3:44])[CH3:43])[N:34]=[CH:33][C:32]=2[O:31][CH2:30][CH2:29]1

참가 물질

5

반응물 3

HCID 10340Sodium CarbonateHCID 578154611,1-Dimethylethyl (2,3-dihydro[1,4]dioxino[2,3-c]pyridin-7-ylmethyl)-4-piperidinylcarbamateHCID 86628365HCID 86628365, 화합물

생성물 1

HCID 86628364HCID 86628364, 화합물수율 52%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a mixture of (7-fluoro-6-hydroxy-3-oxo-5,6-dihydro-3H-pyrrolo[1,2,3-de]quinoxalin-6-yl)methyl 4-methylbenzenesulfonate (0.093 g, 0.24 mmol) in ethanol (3 mL) was added 1,1-dimethylethyl (2,3-dihydro[1,4]dioxino[2,3-c]pyridin-7-ylmethyl)4-piperidinylcarbamate (for a synthesis see WO 2004058144 Example 99(h)) (78.5 mg, 0.22 mmol), then sodium carbonate (71.5 mg, 0.68 mmol). The reaction mixture was stirred at room temperature for 16 hours and evaporated to dryness. The residue was placed directly onto the top of a 20 g silica gel column and chromatographed eluting with a 0-100% ethyl acetate in petrol gradient, then with a 0-50% methanol in ethyl acetate gradient to afford the product (70 mg, 52%).

후처리

  1. customevaporated to dryness
  2. customchromatographed
  3. washeluting with a 0-100% ethyl acetate in petrol gradient

출처 및 근거

ORD 기록
ord-81f7205e1c064573a9785c39836738c2
출처 데이터셋
uspto-grants-2010_05
특허 번호
US07709483B2

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