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Allyl bromide → 9-(8-Allyl-8-aza-bicyclo[3.2.1] oct-3-ylidene)-9H-xanthene-3-carboxylic acid diethylamide

HRID 425280
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HRID 425280 반응식
[CH2:1]([N:3]([CH2:28][CH3:29])[C:4]([C:6]1[CH:7]=[CH:8][C:9]2[C:10](=[C:20]3[CH2:26][CH:25]4[NH:27][CH:22]([CH2:23][CH2:24]4)[CH2:21]3)[C:11]3[C:16]([O:17][C:18]=2[CH:19]=1)=[CH:15][CH:14]=[CH:13][CH:12]=3)=[O:5])[CH3:2].C(=O)([O-])[O-].[K+].[K+].[CH2:36](Br)[CH:37]=[CH2:38]>C(#N)C.O>[CH2:28]([N:3]([CH2:1][CH3:2])[C:4]([C:6]1[CH:7]=[CH:8][C:9]2[C:10](=[C:20]3[CH2:26][CH:25]4[N:27]([CH2:38][CH:37]=[CH2:36])[CH:22]([CH2:23][CH2:24]4)[CH2:21]3)[C:11]3[C:16]([O:17][C:18]=2[CH:19]=1)=[CH:15][CH:14]=[CH:13][CH:12]=3)=[O:5])[CH3:29]
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참가 물질

6

반응물 3

HCID 7841Allyl bromideHCID 11430Potassium CarbonateHCID 469181419-(8-azabicyclo[3.2.1]octan-3-ylidene)-N,N-diethylxanthene-3-carboxamide

생성물 1

HCID 114531349-(8-Allyl-8-aza-bicyclo[3.2.1] oct-3-ylidene)-9H-xanthene-3-carboxylic acid diethylamide수율 26.3%

시약·촉매·용매 2

HCID 962Water용매
HCID 6342
Acetonitrile
용매

실험 절차

To a sample of compound 10a (0.37 g, 0.95 mmol) in 6 mL acetonitrile was added potassium carbonate (0.53 g, 3.81 mmol) and allyl bromide (80 μL, 0.95 mmol). The mixture was stirred at room temperature for 20 h. The reaction was diluted with water and extracted with CH2Cl2. The combined organic extracts were dried over magnesium sulfate and concentrated. The product was purified by flash column chromatography on silica gel, eluting with 10% 0.5 M NH3 in methanol/CH2Cl2 to yield 0.11 g (0.25 mmol) of Compound 14a. The product was converted into its HCl salt using ethereal hydrogen chloride. MS m/z=429.0 (M+1); 1H NMR 300 MHz (CDCl3) δ 1.1-1.4 (m, 6H), 1.7 (m, 2H), 2.3 (m, 2H), 3.1 (m, 2H), 3.4 (m, 2H), 3.6 (m, 4H), 4.0 (m, 2H), 4.4 (m, 2H), 4.7 (m, 2H), 5.5-5.9 (m, 4H), 6.3 (m, 2H), 7.1-7.4 (m, 7H).

후처리

  1. extractionextracted with CH2Cl2
  2. dry with materialThe combined organic extracts were dried over magnesium sulfate
  3. concentrationconcentrated
  4. customThe product was purified by flash column chromatography on silica gel
  5. washeluting with 10% 0.5 M NH3 in methanol/CH2Cl2

출처 및 근거

ORD 기록
ord-1415c58e35294f45b002ffe994ebb1e5
출처 데이터셋
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08106207B2

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