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Hydrochloric Acid → HCID 69550750、化合物

HRID 2214810
ノート
印刷プレビュー

反応式

HRID 2214810 の反応式
I[Si](C)(C)C.C(OC([NH:16][C:17]1([CH2:29][N:30]2[CH2:35][CH2:34][N:33]([S:36]([C:39]3[CH:48]=[CH:47][C:46]4[C:41](=[CH:42][CH:43]=[C:44]([Cl:49])[CH:45]=4)[CH:40]=3)(=[O:38])=[O:37])[CH2:32][C:31]2=[O:50])[CH2:22][CH2:21][N:20]([C:23]2[CH:28]=[CH:27][N:26]=[CH:25][CH:24]=2)[CH2:19][CH2:18]1)=O)C1C=CC=CC=1.CO.[ClH:53]>ClCCl.C(OCC)(=O)C>[ClH:49].[ClH:53].[NH2:16][C:17]1([CH2:29][N:30]2[CH2:35][CH2:34][N:33]([S:36]([C:39]3[CH:48]=[CH:47][C:46]4[C:41](=[CH:42][CH:43]=[C:44]([Cl:49])[CH:45]=4)[CH:40]=3)(=[O:37])=[O:38])[CH2:32][C:31]2=[O:50])[CH2:22][CH2:21][N:20]([C:23]2[CH:24]=[CH:25][N:26]=[CH:27][CH:28]=2)[CH2:19][CH2:18]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 887Methanol2 回HCID 85247Trimethylsilyl iodideHCID 69550015HCID 69550015、化合物

生成物 1

HCID 69550750HCID 69550750、化合物

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒
HCID 8857
Ethyl Acetate
溶媒

実験手順

Iodotrimethylsilane (2.51 ml) was added to a solution of 1-[4-benzyloxycarbonylamino-1-(4-pyridyl)-4-piperidylmethyl]-4-(6-chloronaphthalene-2-sulfonyl)-2-piperazinone (4.58 g) in dichloromethane (50 ml), and the mixture was stirred at room temperature for 4 hours. Methanol (10 ml) and 4N hydrochloric acid solution in ethyl acetate (8 ml) were added thereto. Methanol was added to obtain a solution, followed by concentration under reduced pressure. Dilute hydrochloric acid was added to the residue, and the mixture was washed with ether. The aqueous layer was made basic with 6N sodium hydroxide, followed by extraction with ethyl acetate. The organic layer was washed successively with an aqueous sodium bicarbonate solution and an aqueous saturated sodium chloride solution, dried, and concentrated. Dilute hydrochloric solution was added to the residue, which was purified by CHP20 column chromatography (water:acetonitrile:1N hydrochloric acid=100:0:1→80:20:1) to obtain the colorless amorphous title compound (3.66 g).

後処理

  1. customto obtain a solution
  2. concentrationfollowed by concentration under reduced pressure
  3. additionDilute hydrochloric acid was added to the residue
  4. washthe mixture was washed with ether
  5. extractionfollowed by extraction with ethyl acetate
  6. washThe organic layer was washed successively with an aqueous sodium bicarbonate solution
  7. dry with materialan aqueous saturated sodium chloride solution, dried
  8. concentrationconcentrated
  9. additionDilute hydrochloric solution
  10. additionwas added to the residue, which
  11. customwas purified by CHP20 column chromatography (water:acetonitrile:1N hydrochloric acid=100:0:1→80:20:1)

出典と根拠

ORDレコード
ord-b4d79b17acc44b0a81147ae01c2355ae
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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