HCID 59625273、化合物 → HCID 59625433、化合物

HRID 2192883ノート

反応式

HRID 2192883 の反応式
[N:1]1([C:5]([C@@H:7]2[CH2:12][C@H:11]([N:13]([C:18]([C:20]3[C:21]([NH:30][CH2:31][CH2:32][CH2:33][O:34][CH3:35])=[N:22][C:23]([C:26]([CH3:29])([CH3:28])[CH3:27])=[N:24][CH:25]=3)=[O:19])[CH2:14][CH:15]([CH3:17])[CH3:16])[CH2:10][N:9](C(OC(C)(C)C)=O)[CH2:8]2)=[O:6])[CH2:4][CH2:3][CH2:2]1>C(OCC)(=O)C.Cl>[N:1]1([C:5]([C@H:7]2[CH2:8][NH:9][CH2:10][C@@H:11]([N:13]([CH2:14][CH:15]([CH3:17])[CH3:16])[C:18]([C:20]3[C:21]([NH:30][CH2:31][CH2:32][CH2:33][O:34][CH3:35])=[N:22][C:23]([C:26]([CH3:28])([CH3:29])[CH3:27])=[N:24][CH:25]=3)=[O:19])[CH2:12]2)=[O:6])[CH2:2][CH2:3][CH2:4]1

参加物

3

反応物 1

HCID 59625273HCID 59625273、化合物

生成物 1

HCID 59625433HCID 59625433、化合物収率 42.3%

試薬・触媒・溶媒 1

HCID 21866389Hydrogen chloride-ethyl acetate溶媒

実験手順

tert-Butyl (3R,5S)-3-(azetidin-1-ylcarbonyl)-5-[({2-tert-butyl-4-[(3-methoxypropyl)amino]pyrimidin-5-yl}carbonyl)(2-methylpropyl)amino]piperidine-1-carboxylate (94 mg) was dissolved in 4 M hydrogen chloride-ethyl acetate (3 ml), and the mixture was stirred at room temperature for 3 hr. The reaction mixture was concentrated under reduced pressure, and the residue was subjected to reversed-phase preparative HPLC. Aqueous sodium hydrogen carbonate was added to the object fraction, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure to give the object compound (33 mg).

後処理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. additionAqueous sodium hydrogen carbonate was added to the object fraction
  3. extractionthe mixture was extracted with ethyl acetate
  4. washThe extract was washed with saturated brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. customThe solvent was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-b2376de9f1784561950b8d58e2acc387
出典データセット
uspto-grants-2012_12
特許番号
US08329691B2

反応ノート

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