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Hydrochloric Acid → HCID 69550015、化合物

HRID 2214809
ノート
印刷プレビュー

反応式

HRID 2214809 の反応式
Cl.[CH2:2]([O:9][C:10]([NH:12][C:13]1([CH2:26][N:27]2[CH2:32][CH2:31][N:30]([S:33]([C:36]3[CH:45]=[CH:44][C:43]4[C:38](=[CH:39][CH:40]=[C:41]([Cl:46])[CH:42]=4)[CH:37]=3)(=[O:35])=[O:34])[CH2:29][C:28]2=[O:47])[CH2:18][CH2:17][N:16](C(OC(C)(C)C)=O)[CH2:15][CH2:14]1)=[O:11])[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1>C(OCC)(=O)C.C(O)C>[CH2:2]([O:9][C:10]([NH:12][C:13]1([CH2:26][N:27]2[CH2:32][CH2:31][N:30]([S:33]([C:36]3[CH:45]=[CH:44][C:43]4[C:38](=[CH:39][CH:40]=[C:41]([Cl:46])[CH:42]=4)[CH:37]=3)(=[O:34])=[O:35])[CH2:29][C:28]2=[O:47])[CH2:18][CH2:17][N:16]([C:13]2[CH:18]=[CH:17][N:16]=[CH:15][CH:14]=2)[CH2:15][CH2:14]1)=[O:11])[C:3]1[CH:4]=[CH:5][CH:6]=[CH:7][CH:8]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 695500601-[4-Benzyloxycarbonylamino-1-(tert-butoxycarbonyl)-4-piperidylmethyl]-4-(6-chloronaphthalene-2-sulfonyl)-2-piperazinone

生成物 1

HCID 69550015HCID 69550015、化合物収率 99.9%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 8857Ethyl Acetate溶媒

実験手順

A 4N hydrochloric acid solution in ethyl acetate (50 ml) and ethanol (10 ml) was added to 1-[4-benzyloxycarbonylamino-1-(tert-butoxycarbonyl)-4-piperidylmethyl]-4-(6-chloronaphthalene-2-sulfonyl)-2-piperazinone (7.42 g), and the mixture was stirred at room temperature for 1 hour. The reaction mixture was concentrated under reduced pressure, 4-chloropyridine hydrochloride (1.80 g), triethylamine(6.97 ml) and ethanol (100 ml) were added to the residue, and the mixture was heated at 150° C. for 5 hours in a sealed tube. After cooling, the reaction mixture was diluted with ethyl acetate, and washed with water. The ethyl acetate layer was dried with magnesium sulfate, and concentrated under reduced pressure. The residue was purified by basic silica gel chromatography (ethyl acetate-ethyl acetate/methanol=8/1) to obtain the title compound (3.58 g, 55%) as powders.

後処理

  1. concentrationThe reaction mixture was concentrated under reduced pressure, 4-chloropyridine hydrochloride (1.80 g), triethylamine(6.97 ml) and ethanol (100 ml)
  2. additionwere added to the residue
  3. temperaturethe mixture was heated at 150° C. for 5 hours in a sealed tube
  4. temperatureAfter cooling
  5. additionthe reaction mixture was diluted with ethyl acetate
  6. washwashed with water
  7. dry with materialThe ethyl acetate layer was dried with magnesium sulfate
  8. concentrationconcentrated under reduced pressure
  9. customThe residue was purified by basic silica gel chromatography (ethyl acetate-ethyl acetate/methanol=8/1)

出典と根拠

ORDレコード
ord-755e72ba429b42d0906f523e2ad8672e
出典データセット
uspto-grants-2006_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07109200B2

反応ノート

読み込み中…

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