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Hydrochloric Acid → HCID 86609028、化合物

HRID 2104466
ノート
印刷プレビュー

反応式

HRID 2104466 の反応式
Cl.C([O:6][C:7]([C@H:9]1[CH2:14][CH2:13][C@H:12]([NH:15][C:16](=[S:27])[C:17]([NH:19][C:20]2[CH:25]=[CH:24][C:23]([Cl:26])=[CH:22][N:21]=2)=[O:18])[C@H:11]([NH:28][C:29]([C:31]2[S:32][C:33]3[CH2:34][N:35]([CH3:40])[CH2:36][CH2:37][C:38]=3[N:39]=2)=[O:30])[CH2:10]1)=[O:8])(C)(C)C>O1CCOCC1>[ClH:26].[Cl:26][C:23]1[CH:24]=[CH:25][C:20]([NH:19][C:17](=[O:18])[C:16]([NH:15][C@H:12]2[CH2:13][CH2:14][C@H:9]([C:7]([OH:8])=[O:6])[CH2:10][C@H:11]2[NH:28][C:29]([C:31]2[S:32][C:33]3[CH2:34][N:35]([CH3:40])[CH2:36][CH2:37][C:38]=3[N:39]=2)=[O:30])=[S:27])=[N:21][CH:22]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 57804530HCID 57804530、化合物

生成物 1

HCID 86609028HCID 86609028、化合物収率 170.8%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒2 回

実験手順

4N HCl in dioxane (10 mL) was added to a solution of the compound obtained in Example 377 (293 mg) in dioxane (8.0 mL), and the mixture was stirred for 16 hours at room temperature. The reaction mixture was concentrated under reduced mixture, and the residue was suspended in diisopropyl ether and then collected through filtration. The collected powder was dissolved in water and then neutralized with saturated aqueous sodium bicarbonate. The aqueous solution was extracted with methylene chloride, and the formed organic layer was washed with saturated brine and dried over sodium sulfate anhydrate, followed by concentration under reduced pressure. 1N HCl in ethanol (0.50 mL) was added to the residue, and the mixture was subjected to concentration under reduced pressure. The residue was dissolved in water, followed by freeze-drying, to thereby yield the title compound (242 mg).

後処理

  1. concentrationThe reaction mixture was concentrated under reduced mixture
  2. filtrationcollected through filtration
  3. dissolutionThe collected powder was dissolved in water
  4. extractionThe aqueous solution was extracted with methylene chloride
  5. washthe formed organic layer was washed with saturated brine
  6. dry with materialdried over sodium sulfate anhydrate
  7. concentrationfollowed by concentration under reduced pressure
  8. addition1N HCl in ethanol (0.50 mL) was added to the residue
  9. concentrationthe mixture was subjected to concentration under reduced pressure
  10. dissolutionThe residue was dissolved in water
  11. customby freeze-drying

出典と根拠

ORDレコード
ord-c123174ab84447fc90b3b981ab218323
出典データセット
uspto-grants-2009_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07576135B2

反応ノート

読み込み中…

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