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Sodium Azide → 2-[(S)-1-Phenylethylamino]-4-[5-azidobenzimidazol-1-yl]pyrimidine

HRID 2300810
ノート
印刷プレビュー

反応式

HRID 2300810 の反応式
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]=[CH:26][C:27]([NH2:29])=[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]=[CH:26][C:27]([N:29]=[N+:30]=[N-:31])=[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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

HCID 33557Sodium AzideHCID 98839772-[(S)-1-phenylethylamino]-4-[5-aminobenzimidazol-1-yl]pyrimidineHCID 23668193Sodium Nitrite

生成物 1

HCID 599246482-[(S)-1-Phenylethylamino]-4-[5-azidobenzimidazol-1-yl]pyrimidine収率 87.7%

試薬・触媒・溶媒 3

HCID 176Acetic Acid溶媒
HCID 962
Water
溶媒
2 回
HCID 8857Ethyl Acetate溶媒

反応条件

温度
0 °C

実験手順

A solution of 12 mg of NaNO2 in 0.5 mL of H2O was added to a 5° C. solution of 56 mg of 2-[(S)-1-phenylethylamino]-4-[5-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 16.5 mg 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 53 mg of the title compound. RF: 0.6 (5% MeOH in CH2Cl2). 1H NMR (400 MHz, 1:1 CD3OD/CDCl3): δ 1.60 (d, J=7.0 Hz, 3H), 5.12 (q, J=7.0 Hz, 1H), 6.8 (m, 1H), 6.95 (d, J=6 Hz, 1H), 7.2-7.45 (m, 6H), 7.72 (m, 1H), 8.33 (br s, J=6.5 Hz, 1H), 8.74 (m, 1H). Mass Spectrum (CH3CN-TFA-NH4HCO2-ESI): 357.1 (M+1).

後処理

  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

出典と根拠

ORDレコード
ord-539865523a6b4aff94e595e713499542
出典データセット
uspto-grants-2002_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06498165B1

反応ノート

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