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Ethanol → HCID 18706904, 화합물

HRID 1422085
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HRID 1422085 반응식
[NH:1]1[CH2:5][CH2:4][CH2:3][CH2:2]1.[H-].[Na+].[CH2:8]([O:15][C:16]1[C:17]2[N:18]3[C:22](=[CH:23][CH:24]=1)[C:21]([CH2:25][CH3:26])=[C:20]([C:27]1[CH:32]=[CH:31][C:30]([O:33][CH2:34][C:35]4[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=4)=[CH:29][CH:28]=1)[C:19]3=[C:41]([CH2:43][O:44][CH2:45][CH2:46][CH2:47][CH2:48]Cl)[CH:42]=2)[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1.C(O)C>CN(C)C=O.O.C(OCC)(=O)C>[CH2:8]([O:15][C:16]1[C:17]2[N:18]3[C:22](=[CH:23][CH:24]=1)[C:21]([CH2:25][CH3:26])=[C:20]([C:27]1[CH:32]=[CH:31][C:30]([O:33][CH2:34][C:35]4[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=4)=[CH:29][CH:28]=1)[C:19]3=[C:41]([CH2:43][O:44][CH2:45][CH2:46][CH2:47][CH2:48][N:1]1[CH2:5][CH2:4][CH2:3][CH2:2]1)[CH:42]=2)[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 702EthanolHCID 24758Sodium hydrideHCID 31268PyrrolidineHCID 187069385-Benzyloxy-2-(4-benzyloxyphenyl)-3-((4-chlorobutoxy)methyl)-1-ethylpyrrolo[2,1,5-cd]indolizine

생성물 1

HCID 18706904HCID 18706904, 화합물수율 12.5%

시약·촉매·용매 3

HCID 962
Water
용매
HCID 6228Dimethylformamide용매
HCID 8857Ethyl Acetate용매

실험 절차

Pyrrolidine (66 mg, 0.93 mmol) was dissolved in 50 ml of dry dimethylformamide under a nitrogen atmosphere and sodium hydride (60% in oil) (36 mg, 0.89 mmol) was added. The mixture was stirred for 1/2 hour. 5Benzyloxy-2-(4-benzyloxyphenyl)-3-((4-chlorobutoxy)methyl)-1-ethylpyrrolo[2,1,5-cd]indolizine (0.256 g, 0.443 mmol) was added and the mixture was stirred at 55-65° for 6 days. Ethanol (10 ml) was added dropwise, and the reaction mixture was diluted with 250 ml of water. The organic material was extacted into ethyl acetate (4×100 ml), and the combined oranic layers were washed with brine and dried over sodium solfate. The solvent was evaporated and the crude product was purified by column chromatography over silica gel 60, using 6% of methanol in dichloromethane as the eluent. Fractions containing the product were collected to afford 34 mg (12%) of 5-benzyloxy-2-(4-benzyloxyphenyl)-1-ethyl-3-((4-pyrrolidinobutoxy)methyl)pyrrolo[2,1,5-cd ]indolizine as an oil. MS(FAB): m/z613 (M+1). 1H-NMR (DMSO-d6, 300 MHz) δ: 1.27-1.49 (m, 11H); 2.50-2.56 (m, 6H); 3.05 (q, 2H); 3.40 (t, 2H); 4.71 (s, 2H); 5.20 (s, 2H); 5.58 (s, 2H); 7.20 (d, 2H); 7.31-7.64 (m, 14H); 7.95 (d, 1H).

후처리

  1. stirringthe mixture was stirred at 55-65° for 6 days
  2. washthe combined oranic layers were washed with brine
  3. dry with materialdried over sodium solfate
  4. customThe solvent was evaporated
  5. customthe crude product was purified by column chromatography over silica gel 60
  6. additionFractions containing the product
  7. customwere collected

출처 및 근거

ORD 기록
ord-c54c39e496014976bd7cc32c08cf4436
출처 데이터셋
uspto-grants-2000_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06080754

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