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1,2-Dichloroethane → HCID 178423797、化合物

HRID 1257536
ノート
印刷プレビュー

反応式

HRID 1257536 の反応式
[F:1][C:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[CH:4][C:3]=1[C:9]1[CH:14]=[C:13]([C:15]2[CH2:19][C@@H:18]([C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][N:21]=3)[O:17][N:16]=2)[CH:12]=[C:11]([C:26]([OH:28])=O)[CH:10]=1.Cl.[N:30]1[N:31]=[C:32]([C@@H:35]([NH2:37])[CH3:36])[NH:33][CH:34]=1.C(Cl)CCl.C1C=NC2N(O)N=NC=2C=1.C(N(CC)CC)C>CN(C)C=O.O>[F:1][C:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[CH:4][C:3]=1[C:9]1[CH:14]=[C:13]([C:15]2[CH2:19][C@@H:18]([C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][N:21]=3)[O:17][N:16]=2)[CH:12]=[C:11]([C:26]([NH:37][C@H:35]([C:32]2[NH:33][CH:34]=[N:30][N:31]=2)[CH3:36])=[O:28])[CH:10]=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 111,2-DichloroethaneHCID 8471TriethylamineHCID 181649HOAtHCID 668959112'-fluoro-4'-methyl-5-[(5S)-5-(2-pyridinyl)-4,5-dihydro-3-isoxazolyl]-3-biphenylcarboxylic acidHCID 178462005HCID 178462005、化合物

生成物 1

HCID 178423797HCID 178423797、化合物

試薬・触媒・溶媒

2
HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 2′-fluoro-4′-methyl-5-[(5S)-5-(2-pyridinyl)-4,5-dihydro-3-isoxazolyl]-3-biphenylcarboxylic acid (125 mg, 0.227 mmol) in N,N-dimethylformamide (1 mL) were added (1S)-1-(4H-1,2,4-triazol-3-yl)ethanamine hydrochloride salt (52 mg, 0.283 mmol), EDC (65 mg, 0.340 mmol), HOAT (9 mg, 0.068 mmol) and triethylamine (95 μL, 0.680 mmol). The reaction mixture was stirred at ambient temperature for 18 h. Water was added. Purification by reverse phase HPLC(C-18, 95% water/acetonitrile→5% water/acetonitrile with 0.05% ammonium hydroxide), and concentration gave the free base. Concentrate was taken up in dichloromethane into which hydrogen chloride gas was bubbled. Concentration gave the title compound as the hydrochloride salt (94.0 mg). HRMS 471.1977 (M+1). 1H NMR (500 MHz, CD 30D): δ 8.94 (s, 1H); 8.78 (d, J=5.6 Hz, 1H); 8.53 (t, J=7.7 Hz, 1H); 8.25 (t, J=1.7 Hz, 1H); 8.16 (t, J=1.6 Hz, 1H); 8.11-8.07 (m, 2H); 7.94 (t, J=6.6 Hz, 1H); 7.46 (t, J=7.9 Hz, 1H); 7.15-7.07 (m, 2H); 6.18 (dd, J=11.4, 6.6 Hz, 1H); 5.50-5.45 (m, 1H); 4.21 (dd, J=17.3, 11.5 Hz, 1H); 3.86 (dd, J=20.8, 7.9 Hz, 1H); 2.41 (s, 3H); 1.74 (d, J=7.1 Hz, 3H).

後処理

  1. customPurification by reverse phase HPLC(C-18, 95% water/acetonitrile→5% water/acetonitrile with 0.05% ammonium hydroxide), and
  2. concentrationconcentration
  3. customgave the free base
  4. concentrationConcentrate
  5. customwas bubbled
  6. concentrationConcentration

出典と根拠

ORDレコード
ord-02b8e6b9e2a14a6780af43d54fd565fd
出典データセット
uspto-grants-2013_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08461185B2

反応ノート

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