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Triethylamine → N-(2-Amino-phenyl)-4-{2-[(pyridin-3-ylmethyl)-carbamoyl]-vinyl}-benzamide

HRID 1180803
ノート
印刷プレビュー

反応式

HRID 1180803 の反応式
N1(O[C:11]([CH:13]=[CH:14][C:15]2[CH:24]=[CH:23][C:18]([C:19]([O:21]C)=O)=[CH:17][CH:16]=2)=[O:12])C2C=CC=CC=2N=N1.CCN(CC)CC.CN([P+](O[N:43]1N=[N:50][C:45]2[CH:46]=[CH:47][CH:48]=[CH:49][C:44]1=2)(N(C)C)N(C)C)C.F[P-](F)(F)(F)(F)F.[NH2:59][CH2:60][C:61]1[CH:62]=[N:63][CH:64]=[CH:65][CH:66]=1.[NH4+].[Cl-]>CN(C=O)C.CCOC(C)=O>[NH2:50][C:45]1[CH:46]=[CH:47][CH:48]=[CH:49][C:44]=1[NH:43][C:19](=[O:21])[C:18]1[CH:17]=[CH:16][C:15]([CH:14]=[CH:13][C:11](=[O:12])[NH:59][CH2:60][C:61]2[CH:62]=[N:63][CH:64]=[CH:65][CH:66]=2)=[CH:24][CH:23]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 8471Triethylamine2 回HCID 25517Ammonium ChlorideHCID 310183-PyridinemethanamineHCID 151348Benzotriazol-1-yloxy-tris(dimethylamino)phosphonium hexafluorophosphateHCID 72479810Methyl 4-[2-(benzotriazol-1-yloxycarbonyl)-vinyl]-benzoate

生成物 1

HCID 68976549
N-(2-Amino-phenyl)-4-{2-[(pyridin-3-ylmethyl)-carbamoyl]-vinyl}-benzamide
収率 92%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒2 回HCID 8857Ethyl Acetate溶媒

実験手順

To a stirred solution at room temperature of VIII (140 mg, 0.68 mmol) in anhydrous DMF (5 ml) under nitrogen were added Et3N (104 μl, 0.75 mmol) and BOP reagent (331 mg, 0.75 mmol), respectively. After 30 min, a solution of 3-(aminomethyl)pyridine (90 μl, 0.88 mmol) or R1R2NH (1.2–1.3 equiv.), Et3N (284 μl, 2.04 mmol) in anhydrous DMF (2 ml) was added dropwise. After 4 h, the reaction mixture was poured into a saturated aqueous solution of NH4Cl, and diluted with AcOEt. After separation, the organic layer was successively washed with sat NH4Cl, H2O and brine, dried over MgSO4, filtered, and concentrated. The crude residue was then purified by flash chromatography on silica gel (MeOH/CH2Cl2:5/95→7/93) to afford the title compound IXb (185 mg, 0.62 mmol, 92% yield) as a white solid. 1H NMR (300 MHz, CDCl3) δ(ppm): 8.67–8.44 (m, 2H), AB system (δA=8.03, δB=7.55, J=8.4 Hz, 4H), 7.78–7.64 (m, 2H), 7.33–7.26 (m, 1H), 6.54 (d, J=15.8 Hz, 1H), 6.38 (bs, 1H), 4.61 (d, J=6.2 Hz, 2H), 3.92 (s, 3H).

後処理

  1. waitAfter 4 h
  2. customAfter separation
  3. washthe organic layer was successively washed with sat NH4Cl, H2O and brine
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customThe crude residue was then purified by flash chromatography on silica gel (MeOH/CH2Cl2:5/95→7/93)

出典と根拠

ORDレコード
ord-4dabe5dcbd0248c1a4326d786e4d1009
出典データセット
uspto-grants-2007_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07282608B2

反応ノート

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