Hydrochloric Acid → HCID 178484861, 화합물

HRID 630376노트

반응식

HRID 630376 반응식
[OH:1][C:2]([C:26]1[S:27][CH:28]=[CH:29][CH:30]=1)([C:21]1[S:22][CH:23]=[CH:24][CH:25]=1)[C:3]([O:5][C@H:6]1[CH2:11][CH2:10][C@H:9]([N:12](C(OC(C)(C)C)=O)[CH3:13])[CH2:8][CH2:7]1)=[O:4].Cl>O1CCOCC1>[OH:1][C:2]([C:21]1[S:22][CH:23]=[CH:24][CH:25]=1)([C:26]1[S:27][CH:28]=[CH:29][CH:30]=1)[C:3]([O:5][C@H:6]1[CH2:7][CH2:8][C@H:9]([NH:12][CH3:13])[CH2:10][CH2:11]1)=[O:4]

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 178486063HCID 178486063, 화합물2회

생성물 1

HCID 178484861HCID 178484861, 화합물수율 78%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매2회

실험 절차

To a solution of trans-4-[(tert-butoxycarbonyl)(methyl)amino]cyclohexyl hydroxy(di-2-thienyl)acetate (intermediate 4; 8.1 g, 0.01 mol) in dioxane (13.5 mL) was added hydrogen chloride 4M in dioxane (27 mL). The mixture was stirred at room temperature for 24 hours. The precipitate obtained was filtrated and washed with ether. The crude was dissolved in water and potassium carbonate was added until pH=8-9. The product was extracted with ethyl acetate and the organic layer was washed with brine, dried and evaporated to dryness giving the title compound as a white solid (78%).

후처리

  1. customThe precipitate obtained
  2. filtrationwas filtrated
  3. washwashed with ether
  4. dissolutionThe crude was dissolved in water
  5. additionpotassium carbonate was added until pH=8-9
  6. extractionThe product was extracted with ethyl acetate
  7. washthe organic layer was washed with brine
  8. customdried
  9. customevaporated to dryness

출처 및 근거

ORD 기록
ord-2d8c6416cbac4bb49c7ede0042cd467f
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09315463B2

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