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Isopropylamine → (R)-5-(6-cyclohexyl-1-(hydroxyamino)-1-oxohexan-3-yl)-N-isopropyl-1,2,4-oxadiazole-3-carboxamide

HRID 1279769
ノート
印刷プレビュー

反応式

HRID 1279769 の反応式
[CH:1]1([CH2:7][CH2:8][CH2:9][C@@H:10]([C:15]2[O:19][N:18]=[C:17]([C:20]([O:22]CC)=O)[N:16]=2)[CH2:11][C:12]([OH:14])=O)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[CH:25]([NH2:28])([CH3:27])[CH3:26].CN1CCOCC1.ClC(OCC(C)C)=O.C[Si](C)(C)[O:46][NH2:47].FC(F)(F)C(O)=O>C(O)C.O>[CH:1]1([CH2:7][CH2:8][CH2:9][C@@H:10]([C:15]2[O:19][N:18]=[C:17]([C:20]([NH:28][CH:25]([CH3:27])[CH3:26])=[O:22])[N:16]=2)[CH2:11][C:12]([NH:47][OH:46])=[O:14])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

9

反応物 6

HCID 6363IsopropylamineHCID 6422Trifluoroacetic acidHCID 79724-MethylmorpholineHCID 62365Isobutyl chloroformateHCID 2734666O-(Trimethylsilyl)hydroxylamineHCID 59909750(3R)-6-cyclohexyl-3-[3-(ethoxycarbonyl)-1,2,4-oxadiazol-5-yl]hexanoic acid

生成物 1

HCID 9947332
(R)-5-(6-cyclohexyl-1-(hydroxyamino)-1-oxohexan-3-yl)-N-isopropyl-1,2,4-oxadiazole-3-carboxamide
収率 8%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒2 回HCID 962Water溶媒

反応条件

温度
80 °C

実験手順

A solution of (3R)-6-cyclohexyl-3-[3-(ethoxycarbonyl)-1,2,4-oxadiazol-5-yl]hexanoic acid (Preparation 4) (500 mg, 1.47 mmol) in ethanol (13 ml) was treated with a solution of isopropylamine (434 mg, 7.35 mmol) in ethanol (2 ml) and the resulting mixture was heated at 80° C. under a nitrogen atmosphere for 10 hours. The solvent was removed under reduced pressure and the residue was dissolved in hydrochloric acid (1M, 10 ml) then extracted with ethyl acetate (×2). The combined organic layers were dried over anhydrous magnesium sulphate, filtered and the solvent removed under reduced pressure. This residue (531 mg) was then dissolved in dichloromethane (15 ml), cooled to 0° C. and treated sequentially with N-methylmorpholine (180 μl, 1.63 mmol) and isobutyl chloroformate (210 μl, 1.62 mmol). This mixture was stirred at 0° C. under a nitrogen atmosphere for 1 hour, then treated with O-(trimethylsilyl)hydroxylamine (220 μl, 1.80 mmol) and stirring continued for 10 minutes at 0° then for 17 hours at room temperature. The mixture was then treated with trifluoroacetic acid:water (5 ml, 9:1) and the solution stirred for 30 minutes. The solvent was removed under reduced pressure and the residue azeotroped from toluene (×2). The residue was purified by reverse phase HPLCa to afford the title compound as a foam (43 mg).

後処理

  1. customThe solvent was removed under reduced pressure
  2. dissolutionthe residue was dissolved in hydrochloric acid (1M, 10 ml)
  3. extractionthen extracted with ethyl acetate (×2)
  4. dry with materialThe combined organic layers were dried over anhydrous magnesium sulphate
  5. filtrationfiltered
  6. customthe solvent removed under reduced pressure
  7. dissolutionThis residue (531 mg) was then dissolved in dichloromethane (15 ml)
  8. temperaturecooled to 0° C.
  9. stirringstirring
  10. waitcontinued for 10 minutes at 0°
  11. waitfor 17 hours at room temperature
  12. customThe solvent was removed under reduced pressure
  13. customthe residue azeotroped from toluene (×2)
  14. customThe residue was purified by reverse phase HPLCa

出典と根拠

ORDレコード
ord-0471903d554b443aa2efc1609f61d6be
出典データセット
uspto-grants-2002_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06448278B2

反応ノート

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