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Hydrochloric Acid → HCID 22901902, 화합물

HRID 1735989
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HRID 1735989 반응식
C(OC([O:6][CH:7]1[C:12]2[CH:13]=[C:14]([S:16]([NH:19][C:20]([CH3:23])([CH3:22])[CH3:21])(=[O:18])=[O:17])[S:15][C:11]=2[S:10](=[O:25])(=[O:24])[N:9](C(OCC)C)[CH2:8]1)C)C.Cl>C1COCC1>[OH:6][CH:7]1[C:12]2[CH:13]=[C:14]([S:16]([NH:19][C:20]([CH3:21])([CH3:22])[CH3:23])(=[O:17])=[O:18])[S:15][C:11]=2[S:10](=[O:25])(=[O:24])[NH:9][CH2:8]1
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참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 19434048HCID 19434048, 화합물

생성물 1

HCID 22901902HCID 22901902, 화합물수율 75%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A mixture of the product from Step E (158 g, 0.325 mol), THF (700 mL) and 2N HCl (180 mL) were stirred at room temperature for 20 hr. After evaporating the THF, the aqueous mixture was cooled to 0° C. and sodium bicarbonate (50 g) was carefully added followed by water (400 mL) and ethyl acetate (500 mL). The two layers were separated and the aqueous layer was extracted with ethyl acetate (250 mL). The combined organic extracts were washed with brine, dried (MgSO4) and evaporated to give a foam which was triturated with methylene chloride (200 mL) to give a solid (81.7 g, 75%): mp 144°-147° C. Recrystallization of this solid from methylene chloride gave an off-white solid: mp 163°-165° C.

후처리

  1. customAfter evaporating the THF
  2. temperaturethe aqueous mixture was cooled to 0° C.
  3. additionsodium bicarbonate (50 g) was carefully added
  4. customThe two layers were separated
  5. extractionthe aqueous layer was extracted with ethyl acetate (250 mL)
  6. washThe combined organic extracts were washed with brine
  7. dry with materialdried (MgSO4)
  8. customevaporated
  9. customto give a foam which
  10. customwas triturated with methylene chloride (200 mL)

출처 및 근거

ORD 기록
ord-f13e86aa1547499ea35d5ee6ccdd715c
출처 데이터셋
uspto-grants-1996_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05538966

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