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Triethylamine → HCID 178471797、化合物

HRID 505312
ノート
印刷プレビュー

反応式

HRID 505312 の反応式
[CH2:1]([O:3][C:4](=[O:15])[CH2:5][C@H:6]1[CH2:11][CH2:10][C@H:9]([C:12]([OH:14])=O)[CH2:8][CH2:7]1)[CH3:2].C(Cl)(=O)C(Cl)=O.[NH2:22][C:23]1[CH:50]=[CH:49][C:48]([O:51][C:52]([F:55])([F:54])[F:53])=[CH:47][C:24]=1[CH2:25][N:26]1[C@@H:30]([CH3:31])[C@@H:29]([C:32]2[CH:37]=[C:36]([C:38]([F:41])([F:40])[F:39])[CH:35]=[C:34]([C:42]([F:45])([F:44])[F:43])[CH:33]=2)[O:28][C:27]1=[O:46].C(N(CC)CC)C>C1COCC1.CN(C=O)C>[F:45][C:42]([F:43])([F:44])[C:34]1[CH:33]=[C:32]([C@H:29]2[O:28][C:27](=[O:46])[N:26]([CH2:25][C:24]3[CH:47]=[C:48]([O:51][C:52]([F:53])([F:54])[F:55])[CH:49]=[CH:50][C:23]=3[NH:22][C:12]([C@H:9]3[CH2:8][CH2:7][C@H:6]([CH2:5][C:4]([O:3][CH2:1][CH3:2])=[O:15])[CH2:11][CH2:10]3)=[O:14])[C@H:30]2[CH3:31])[CH:37]=[C:36]([C:38]([F:39])([F:41])[F:40])[CH:35]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 8471TriethylamineHCID 65578Oxalyl chlorideHCID 57617867(4S,5R)-3-[2-amino-5-(trifluoromethoxy)benzyl]-5-[3,5-bis(trifluoromethyl)phenyl]-4-methyl-1,3-oxazolidin-2-oneHCID 178471800HCID 178471800、化合物

生成物 1

HCID 178471797HCID 178471797、化合物

試薬・触媒・溶媒 2

HCID 6228
Dimethylformamide
溶媒
HCID 8028Tetrahydrofuran溶媒

実験手順

A stirred solution of trans-4-(2-ethoxy-2-oxoethyl)-cyclohexanecarboxylic acid (1 g; 4.67 mmol) in anhydrous THF (25 mL) at 0° C. was treated dropwise with oxalyl chloride (1.02 mL; 11.68 mmol) followed by catalytic DMF (50 μL). The reaction was stirred at room temperature for 2 h, concentrated in vacuo, and the residue was redissolved in THF (25 mL). The resultant solution was cooled to 0° C. and treated with (4S,5R)-3-[2-amino-5-(trifluoromethoxy)benzyl]-5-[3,5-bis(trifluoromethyl)phenyl]-4-methyl-1,3-oxazolidin-2-one (2.58 g; 5.14 mmol) and triethylamine (0.716 mL; 5.14 mmol). The reaction was stirred at room temperature for 1 h, quenched with water and partitioned between EtOAc (100 mL) and H2O (100 mL). The aqueous layer was extracted with EtOAc (3×100 mL) and the combined extracts were washed with brine (100 mL), dried (MgSO4), filtered and concentrated in vacuo. The residue was purified by flash silica gel chromatography, eluting with EtOAc/hexanes, to afford ethyl [trans-4-({[2-({(4S,5R)-5-[3,5-bis(trifluoromethyl)phenyl]-4-methyl-2-oxo-1,3-oxazolidin-3-yl}methyl)-4-(trifluoromethoxy)phenyl]amino}carbonyl)cyclohexyl]acetate as an off-white solid. LCMS=698.9 (M+1)+. 1H NMR (CDCl3, 500 MHz): δ 8.94 (s, 1 H), 8.23 (d, J=8.9 Hz, 1 H), 7.92 (s, 1 H), 7.73 (s, 2H), 7.27-7.24 (m, 1 H), 7.02 (s, 1 H), 5.71 (d, J=8.4 Hz, 1 H), 4.78 (d, J=15.5 Hz, 1 H), 4.19-4.12 (m, 3H), 4.07 (d, J=15.6 Hz, 1 H), 2.43-2.37 (m, 1 H), 2.21 (d, J=6.9 Hz, 2 H), 2.07-1.98 (m, 2 H), 1.93-1.83 (m, 3 H), 1.67 (q, J=12.6 Hz, 2 H), 1.26 (t, J=7.2 Hz, 3 H), 1.19-1.11 (m, 2 H), 0.88 (d, J=6.6 Hz, 3 H).

後処理

  1. concentrationconcentrated in vacuo
  2. dissolutionthe residue was redissolved in THF (25 mL)
  3. temperatureThe resultant solution was cooled to 0° C.
  4. stirringThe reaction was stirred at room temperature for 1 h
  5. customquenched with water
  6. custompartitioned between EtOAc (100 mL) and H2O (100 mL)
  7. extractionThe aqueous layer was extracted with EtOAc (3×100 mL)
  8. washthe combined extracts were washed with brine (100 mL)
  9. dry with materialdried (MgSO4)
  10. filtrationfiltered
  11. concentrationconcentrated in vacuo
  12. customThe residue was purified by flash silica gel chromatography
  13. washeluting with EtOAc/hexanes

出典と根拠

ORDレコード
ord-4cc2b7b07606497b951580fb536078ba
出典データセット
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07781426B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート