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Triphenylphosphine → (1S)-3-[5-(1-Amino-2-biphenyl-4-yl-ethyl)-tetrazol-1-yl]-propionitrile

HRID 333354
ノート
印刷プレビュー

反応式

HRID 333354 の反応式
[C:1]1([C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)[CH:6]=[CH:5][C:4]([CH2:7][C@H:8]([NH:16]C(=O)OC(C)(C)C)[C:9]([NH:11][CH2:12][CH2:13][C:14]#[N:15])=O)=[CH:3][CH:2]=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.CC(OC(/N=N/C(OC(C)C)=O)=O)C.[Si]([N:67]=[N+:68]=[N-:69])(C)(C)C>C1COCC1>[NH2:16][C@H:8]([C:9]1[N:11]([CH2:12][CH2:13][C:14]#[N:15])[N:69]=[N:68][N:67]=1)[CH2:7][C:4]1[CH:5]=[CH:6][C:1]([C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)=[CH:2][CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 11776Triphenylphosphine3 回HCID 78378Azidotrimethylsilane3 回HCID 5363146Diisopropyl azodicarboxylate3 回HCID 53856625(S)-2-t-butoxycarbonylamino-3-biphenyl-4-yl-N-(2-cyanoethyl)-propionamide

生成物 1

HCID 22849544(1S)-3-[5-(1-Amino-2-biphenyl-4-yl-ethyl)-tetrazol-1-yl]-propionitrile収率 73.3%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of (S)-tert-butyl 3-(biphenyl-4-yl)-1-(2-cyanoethylamino)-1-oxopropan-2-ylcarbamate (563 mg, 1.431 mmol) and triphenylphosphine (450 mg, 1.717 mmol) in THF (10 mL) were added DIAD (0.334 mL, 1.717 mmol) and TMSN3 (0.228 mL, 1.717 mmol) at room temperature. After 2 hours, additional triphenylphosphine (180 mg, 0.687 mmol), DIAD (0.134 mL, 0.687 mmol) and TMSN3 (0.0912 mL, 0.687 mmol) were added. After being stirred overnight, additional triphenylphosphine (180 mg, 0.687 mmol), DIAD (0.134 mL, 0.687 mmol) and TMSN3 (0.0912 mL, 0.687 mmol) were added. After being additional 3 hours, the reaction mixture was concentrated and purified by silica gel flash column chromatography (eluent; EtOAc/heptane). The obtained product was treated with 4M HCl in dioxane (10 mL) at room temperature. After being stirred for 1 hour, the reaction mixture was concentrated. The residue was diluted with EtOAc, washed with saturated NaHCO3aq and brine. The organic layer was dried over Na2SO4, concentrated and purified by silica gel flash column chromatography (eluent; MeOH/DCM) to give (S)-3-(5-(1-amino-2-(biphenyl-4-yl)ethyl)-1H-tetrazol-1-yl)propanenitrile (334 mg). 1H NMR (400 MHz, CHLOROFORM-d) δ ppm 2.83 (dt, J=6.82, 16.9 Hz, 1H), 2.96 (dt, J=6.82, 13.89 Hz, 1H), 3.21 (dd, J=8.08, 13.64 Hz, 1H), 3.42 (dd, J=6.06, 13.64 Hz, 1H), 4.47-4.59 (m, 2H), 4.60-4.68 (m, 1H), 7.21 (d, J=8.08 Hz, 2H), 7.33-7.39 (m, 1H), 7.42-7.48 (bt, 2H), 7.54-7.60 (m, 3H).

後処理

  1. waitAfter being additional 3 hours
  2. concentrationthe reaction mixture was concentrated
  3. custompurified by silica gel flash column chromatography (eluent; EtOAc/heptane)
  4. additionThe obtained product was treated with 4M HCl in dioxane (10 mL) at room temperature
  5. stirringAfter being stirred for 1 hour
  6. concentrationthe reaction mixture was concentrated
  7. additionThe residue was diluted with EtOAc
  8. washwashed with saturated NaHCO3aq and brine
  9. dry with materialThe organic layer was dried over Na2SO4
  10. concentrationconcentrated
  11. custompurified by silica gel flash column chromatography (eluent; MeOH/DCM)

出典と根拠

ORDレコード
ord-4e981db7539c42d28c534a922b6afafc
出典データセット
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08877815B2

反応ノート

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