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Sodium Azide → 2-[(S)-1-Phenylethylamino]-4-[6-azidobenzimidazol-1-yl]pyrimidine

HRID 2300811
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HRID 2300811 반응식
N([O-])=O.[Na+].[C:5]1([C@@H:11]([NH:13][C:14]2[N:19]=[C:18]([N:20]3[C:24]4[CH:25]=[C:26]([NH2:29])[CH:27]=[CH:28][C:23]=4[N:22]=[CH:21]3)[CH:17]=[CH:16][N:15]=2)[CH3:12])[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1.[N-:30]=[N+:31]=[N-].[Na+]>O.C(O)(=O)C.C(OCC)(=O)C>[C:5]1([C@@H:11]([NH:13][C:14]2[N:19]=[C:18]([N:20]3[C:24]4[CH:25]=[C:26]([N:29]=[N+:30]=[N-:31])[CH:27]=[CH:28][C:23]=4[N:22]=[CH:21]3)[CH:17]=[CH:16][N:15]=2)[CH3:12])[CH:6]=[CH:7][CH:8]=[CH:9][CH:10]=1
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참가 물질

7

반응물 3

HCID 33557Sodium AzideHCID 98188992-[(S)-1-phenylethylamino]-4-[6-aminobenzimidazol-1-yl]pyrimidineHCID 23668193Sodium Nitrite

생성물 1

HCID 599246882-[(S)-1-Phenylethylamino]-4-[6-azidobenzimidazol-1-yl]pyrimidine수율 73.7%

시약·촉매·용매 3

HCID 176Acetic Acid용매
HCID 962
Water
용매
2회
HCID 8857Ethyl Acetate용매

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온도
0 °C

실험 절차

A solution of 16.3 mg of NaNO2 in 0.5 mL of H2O was added to a 5° C. solution of 78 mg of 2-[(S)-1-phenylethylamino]-4-[6-aminobenzimidazol-1-yl]pyrimidine in 2 mL acetic acid. The solution was cooled to 0° C. and stirred for 0.5 hours. A solution of 23 mg of NaN3 in 0.5 mL H2O was added and stirred for one hour. The solution was diluted with 100 mL of ethyl acetate and washed with water, saturated NaHCO3 and brine. The organic phase was dried over MgSO4, filtered and concentrated under reduced pressure. The residue was purified by flash chromatography eluting with methanol in methylene chloride to give 62 mg of the title compound. RF: 0.6 (5% MeOH in CH2Cl2). 1H NMR (300 MHz, CD3OD): δ1.57 (d, J=7 Hz, 3H), 5.18 (q, J=8 Hz, 1H), 6.88 (d, J=6 Hz, 1H), 7.05 (dd, J=2.5, 9 Hz, 1H), 7.18 (m, 1H), 7.29 (t, J=6 Hz, 2H), 7.43 (d, J=9 Hz, 2H), 7.65 (d, J=9 Hz, 1H), 8.02 (m, 1H), 8.3 (d, J=6 Hz, 1H), 8.69 (b s, 1H). Mass Spectrum (CH3CN-TFA-NH4HCO2-ESI): 357.2 (M+1).

후처리

  1. stirringstirred for one hour
  2. washwashed with water, saturated NaHCO3 and brine
  3. dry with materialThe organic phase was dried over MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was purified by flash chromatography
  7. washeluting with methanol in methylene chloride

출처 및 근거

ORD 기록
ord-4d4bb7cd158440c09144ad9f76ae622d
출처 데이터셋
uspto-grants-2002_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06498165B1

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