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Diisopropylethylamine → HCID 57920097、化合物

HRID 19377
ノート
印刷プレビュー

反応式

HRID 19377 の反応式
[OH:1][C:2]([CH3:26])([CH3:25])[CH2:3][C:4]1[CH:5]=[C:6]([CH:22]=[CH:23][CH:24]=1)[O:7][C:8]1[CH2:12][N:11]([C@@H:13]([CH2:17][CH:18]([CH3:20])[CH3:19])[C:14](O)=[O:15])[C:10](=[O:21])[CH:9]=1.[CH3:27][C:28]1([CH3:40])[O:32][C@H:31]([CH2:33][N:34]2[CH:38]=[CH:37][C:36]([NH2:39])=[N:35]2)[CH2:30][O:29]1.C(N(CC)C(C)C)(C)C.F[P-](F)(F)(F)(F)F.N1(O[P+](N(C)C)(N(C)C)N(C)C)C2C=CC=CC=2N=N1>CN(C)C=O>[CH3:27][C:28]1([CH3:40])[O:32][C@H:31]([CH2:33][N:34]2[CH:38]=[CH:37][C:36]([NH:39][C:14](=[O:15])[C@@H:13]([N:11]3[CH2:12][C:8]([O:7][C:6]4[CH:22]=[CH:23][CH:24]=[C:4]([CH2:3][C:2]([OH:1])([CH3:25])[CH3:26])[CH:5]=4)=[CH:9][C:10]3=[O:21])[CH2:17][CH:18]([CH3:20])[CH3:19])=[N:35]2)[CH2:30][O:29]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 81531DiisopropylethylamineHCID 151348Benzotriazol-1-yloxy-tris(dimethylamino)phosphonium hexafluorophosphateHCID 59344941(R)-1-((2,2-Dimethyl-1,3-dioxolan-4-yl)methyl)-1H-pyrazol-3-amineHCID 66895240HCID 66895240、化合物

生成物 1

HCID 57920097HCID 57920097、化合物収率 76.1%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of (S)-2-{4-[3-(2-hydroxy-2-methyl-propyl)-phenoxy]-2-oxo-2,5-dihydro-pyrrol-1-yl}-4-methyl-pentanoic acid (prepared as in Example 235, 0.159 g, 0.44 mmol) in N,N-dimethylformamide (5 mL) was added 1-((R)-2,2-dimethyl-[1,3]dioxolan-4-yl-methyl)-1H-pyrazol-3-ylamine (prepared as in Example 49, 0.129 g, 0.65 mmol), N,N-diisopropylethylamine (0.312 g, 2.41 mmol) and benzotriazol-1-yl-oxy-tris(dimethylamino)phosphonium hexafluorophosphate (0.778 g, 1.76 mmol) at 0° C. The mixture was allowed to slowly warm up to room temperature and stirred for 48 h. The solvents were then concentrated in vacuo. The residue was dissolved in ethyl acetate and the mixture formed was washed with aqueous saturated ammonium chloride and brine, dried over sodium sulfate, filtered and concentrated in vacuo. The residue was initially purified by flash column chromatography (silica gel 10% to 100% ethyl acetate/hexanes). Then followed by reverse phase HPLC (C18, 20×150 mm column and 45-100% water/acetonitrile gradient at a flow rate of 30 mL/min) to afford (S)-2-{4-[3-(2-hydroxy-2-methyl-propyl)-phenoxy]-2-oxo-2,5-dihydro-pyrrol-1-yl}-4-methyl-pentanoic acid [1-((R)-2,2-dimethyl-[1,3]dioxolan-4-ylmethyl)-1H-pyrazol-3-yl]-amide (0.181 g, 76%) as a white solid: HR-ES-MS m/z calculated for C29H40N4O6 [M+H]+ 541.3021, observed 541.3017; 1H NMR (300 MHz, DMSO-d6) δ ppm 0.89 (d, J=6.3 Hz, 3H), 0.93 (d, J=6.3 Hz, 3H), 1.05 (s, 6H), 1.24 (s, 3H), 1.29 (s, 3H), 1.36-1.64 (m, 2H), 1.63-1.80 (m, 1H), 2.67 (s, 2H), 3.73 (dd, J=8.4, 5.9 Hz, 1H), 4.00 (dd, J=8.4, 6.3 Hz, 1H), 4.03-4.14 (m, 2H), 4.17 (d, J=18.4 Hz, 1H), 4.28-4.37 (m, 1H), 4.36 (s, 1H), 4.55 (d, J=18.4 Hz, 1H), 4.82 (s, 1H), 4.87 (dd, J=10.7, 4.7 Hz, 1H), 6.43 (d, J=2.1 Hz, 1H), 7.03-7.17 (m, 3H), 7.24-7.41 (m, 1H), 7.59 (d, J=2.1 Hz, 1H), 10.77 (s, 1H).

後処理

  1. concentrationThe solvents were then concentrated in vacuo
  2. dissolutionThe residue was dissolved in ethyl acetate
  3. customthe mixture formed
  4. washwas washed with aqueous saturated ammonium chloride and brine
  5. dry with materialdried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo
  8. customThe residue was initially purified by flash column chromatography (silica gel 10% to 100% ethyl acetate/hexanes)

出典と根拠

ORDレコード
ord-4de7af8194284844946c56716bbb5db8
出典データセット
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07741327B2

反応ノート

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