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Toluene → HCID 178453339, 화합물

HRID 870589
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HRID 870589 반응식
[Na].O=C1O[C@H]([C@H](CO)O)C(O)=C1O.[CH2:14]([N:18]([CH2:26][C:27]([N:29]1[CH2:48][CH2:47][C:32]2[N:33]=[C:34]([NH:37][CH:38]3[CH2:46][C:45]4[C:40](=[CH:41][CH:42]=[CH:43][CH:44]=4)[CH2:39]3)[N:35]=[CH:36][C:31]=2[CH2:30]1)=[O:28])[C:19](=[O:25])[O:20][C:21]([CH3:24])([CH3:23])[CH3:22])[CH2:15][C:16]#[CH:17].C1(C)C=CC=CC=1.[N:56]([Si](C)(C)C)=[N+:57]=[N-:58]>CN(C)C=O.O.C(OCC)(=O)C.O.O.O.O.O.S([O-])([O-])(=O)=O.[Cu+2]>[CH2:39]1[C:40]2[C:45](=[CH:44][CH:43]=[CH:42][CH:41]=2)[CH2:46][CH:38]1[NH:37][C:34]1[N:35]=[CH:36][C:31]2[CH2:30][N:29]([C:27](=[O:28])[CH2:26][N:18]([CH2:14][CH2:15][C:16]3[N:56]=[N:57][NH:58][CH:17]=3)[C:19](=[O:25])[O:20][C:21]([CH3:24])([CH3:23])[CH3:22])[CH2:48][CH2:47][C:32]=2[N:33]=1
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참가 물질

9

반응물 4

HCID 1140TolueneHCID 78378AzidotrimethylsilaneHCID 66586226sodium L-ascorbic acidHCID 86726552tert-butyl N-but-3-ynyl-N-[2-[2-(indan-2-ylamino)-7,8-dihydro-5H-pyrido[4,3-d]pyrimidin-6-yl]-2-oxo-ethyl]carbamate

생성물 1

HCID 178453339HCID 178453339, 화합물수율 63.3%

시약·촉매·용매 4

HCID 24463
Copper sulfate pentahydrate
촉매
HCID 962Water용매2회
HCID 6228Dimethylformamide용매
HCID 8857Ethyl Acetate용매

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온도
90 °C

실험 절차

Add copper(II)sulfate pentahydrate (0.026 g; 0.2 equiv; 0.106 mmoles) and L-ascorbic acid sodium salt (0.21 g; 2.0 equiv; 1.06 mmoles) to a deoxygenated solution of tert-butyl N-but-3-ynyl-N-[2-[2-(indan-2-ylamino)-7,8-dihydro-5H-pyrido[4,3-d]pyrimidin-6-yl]-2-oxo-ethyl]carbamate (0.252 g; 1.0 equiv; 0.53 mmoles) in dimethylformamide (6 mL) and water (3 mL) (including toluene (0.05 mL) as an internal standard). Heat the reaction vessel to 90° C. and then add azidotrimethylsilane (0.565 mL; 8 equiv; 4.24 mmoles) slowly. Stir at 90° C. for 4 hours, then dilute the reaction mixture with water (100 mL) and ethyl acetate (50 mL), and extract 3×50 mL ethyl acetate. Wash the combined organic extracts with brine, dry over magnesium sulfate, filter, and concentrate. Purify the crude product by column chromatography (0 to 10% methanol in ethyl acetate) to give tert-butyl {2-[2-(2,3-dihydro-1H-inden-2-ylamino)-7,8-dihydropyrido[4,3-d]pyrimidin-6(5H)-yl]-2-oxoethyl}[2-(1H-1,2,3-triazol-4-yl)-ethyl]carbamate (0.174 g; 63%) as a colorless foam: MS (m/z): 519 (M+1).

후처리

  1. extractionextract 3×50 mL ethyl acetate
  2. washWash the combined organic extracts with brine
  3. dry with materialdry over magnesium sulfate
  4. filtrationfilter
  5. concentrationconcentrate
  6. customPurify the crude product by column chromatography (0 to 10% methanol in ethyl acetate)

출처 및 근거

ORD 기록
ord-807e6e7eb6c84947bd27e8c3e1ad1da6
출처 데이터셋
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08969555B2

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