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Hydrochloric Acid → HCID 86609028, 화합물

HRID 2104466
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HRID 2104466 반응식
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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 57804530HCID 57804530, 화합물

생성물 1

HCID 86609028HCID 86609028, 화합물수율 170.8%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매2회

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-c123174ab84447fc90b3b981ab218323
출처 데이터셋
uspto-grants-2009_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07576135B2

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