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Hydrochloric Acid → HCID 58484014、化合物

HRID 2368077
ノート
印刷プレビュー

反応式

HRID 2368077 の反応式
[CH:1]1([CH2:4][O:5][C:6]2[CH:25]=[CH:24][C:9]3[N:10]=[C:11]([N:13]4[CH2:18][CH2:17][CH:16]([O:19][CH2:20][C:21](=O)[CH3:22])[CH2:15][CH2:14]4)[O:12][C:8]=3[CH:7]=2)[CH2:3][CH2:2]1.[O:26]1[CH:30]=[CH:29][C:28]([NH2:31])=[N:27]1.[B][B][B][B][B][B][B][B][B][B].Cl>CO.C(O)(=O)C>[CH:1]1([CH2:4][O:5][C:6]2[CH:25]=[CH:24][C:9]3[N:10]=[C:11]([N:13]4[CH2:18][CH2:17][CH:16]([O:19][CH2:20][CH:21]([NH:31][C:28]5[CH:29]=[CH:30][O:26][N:27]=5)[CH3:22])[CH2:15][CH2:14]4)[O:12][C:8]=3[CH:7]=2)[CH2:3][CH2:2]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 313Hydrochloric AcidHCID 18102163-IsoxazolamineHCID 67448291HCID 67448291、化合物HCID 178419135HCID 178419135、化合物

生成物 1

HCID 58484014HCID 58484014、化合物

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒
HCID 887
Methanol
溶媒

実験手順

To a solution of 1-({1-[6-(cyclopropylmethoxy)-1,3-benzoxazol-2-yl]piperidin-4-yl}oxy)propan-2-one (400 mg) and isoxazol-3-amine (0.129 mL) in methanol (6 mL) and acetic acid (0.300 mL) was added decaborane (213 mg), and the mixture was stirred at room temperature for 3 hr. 1M Hydrochloric acid was added to the reaction mixture, and the mixture was stirred at room temperature for 30 min, and extracted with ethyl acetate. The extract was washed with saturated brine and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure and the residue was purified by silica gel chromatography (hexane/ethyl acetate). The obtained residue was applied to preparative HPLC (C18, mobile phase: water/acetonitrile (containing 0.1% TFA)). Saturated aqueous sodium hydrogen carbonate solution was added to the obtained fraction, and the mixture was extracted with ethyl acetate and the extract was dried over anhydrous sodium sulfate. The residue was concentrated under reduced pressure to give the title compound (126 mg).

後処理

  1. stirringthe mixture was stirred at room temperature for 30 min
  2. extractionextracted with ethyl acetate
  3. washThe extract was washed with saturated brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. customThe solvent was evaporated under reduced pressure
  6. customthe residue was purified by silica gel chromatography (hexane/ethyl acetate)
  7. additionSaturated aqueous sodium hydrogen carbonate solution was added to the obtained fraction
  8. extractionthe mixture was extracted with ethyl acetate
  9. dry with materialthe extract was dried over anhydrous sodium sulfate
  10. concentrationThe residue was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-8e4e4bb52c954f8bb543fe7c83bf27db
出典データセット
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08703758B2

反応ノート

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