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Hydrochloric Acid → HCID 57971602, 화합물

HRID 2360662
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HRID 2360662 반응식
[CH:1]1([O:6][C:7](=[O:33])[C@@H:8]([NH:16][CH2:17][C:18]2[CH:23]=[CH:22][C:21]([CH2:24][NH:25]C(OC(C)(C)C)=O)=[CH:20][CH:19]=2)[CH2:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[CH2:5][CH2:4][CH2:3][CH2:2]1.Cl.O1CCOCC1>>[CH:1]1([O:6][C:7](=[O:33])[C@@H:8]([NH:16][CH2:17][C:18]2[CH:19]=[CH:20][C:21]([CH2:24][NH2:25])=[CH:22][CH:23]=2)[CH2:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[CH2:2][CH2:3][CH2:4][CH2:5]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 57971739HCID 57971739, 화합물

생성물 1

HCID 57971602HCID 57971602, 화합물수율 79%

실험 절차

(S)-2-[4-(tert-Butoxycarbonylamino-methyl)-benzylamino]-3-phenyl-propionic acid cyclopentyl ester was treated with 4M HCl in dioxane (1 mL, 0.25 mmol) and stirred at r.t. for 1 h. The mixture was evaporated to dryness and partitioned between EtOAc (20 mL) and water (20 mL). Saturated sodium bicarbonate (20 mL) was added to the aqueous layer which was then extracted with EtOAc (3×20 mL). The organic layers were combined, dried (Na2SO4) and evaporated to dryness to give the desired product (263 mg, 79% over 2 steps). m/z 353 [M++H]+

후처리

  • customThe mixture was evaporated to dryness
  • custompartitioned between EtOAc (20 mL) and water (20 mL)
  • additionSaturated sodium bicarbonate (20 mL) was added to the aqueous layer which
  • extractionwas then extracted with EtOAc (3×20 mL)
  • dry with materialdried (Na2SO4)
  • customevaporated to dryness
  • 출처 및 근거

    ORD 기록
    ord-914f824bb2df47c8ae060361396fb6c7
    출처 데이터셋
    uspto-grants-2014_04
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US08686032B2

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