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Hydrogen chloride-ethyl acetate → HCID 68935247, 화합물

HRID 1260926
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HRID 1260926 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([C@H:9]2[C@H:14]([N:15]([CH3:24])[C:16]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)=[O:17])[CH2:13][CH2:12][N:11](C(OC(C)(C)C)=O)[CH2:10]2)[CH:5]=[CH:6][C:7]=1[Cl:8].Cl.C(OCC)(=O)C>C(OCC)(=O)C>[Cl:1][C:2]1[CH:3]=[C:4]([C@H:9]2[C@H:14]([N:15]([CH3:24])[C:16](=[O:17])[C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)[CH2:13][CH2:12][NH:11][CH2:10]2)[CH:5]=[CH:6][C:7]=1[Cl:8]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 21866389Hydrogen chloride-ethyl acetateHCID 86631305rel-1,1-Dimethylethyl (3R,4R)-4-(benzoylmethylamino)-3-(3,4-dichlorophenyl)-1-piperidinecarboxylate

생성물 1

HCID 68935247HCID 68935247, 화합물수율 75.7%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

To a solution of the compound (0.455 g) obtained in Example 13 in ethyl acetate (3 mL) was added 4N hydrogen chloride/ethyl acetate solution (3 mL), and the mixture was stirred at room temperature for 24 hr with heating. The reaction mixture was concentrated under reduced pressure, ethyl acetate was added to the residue, and the mixture was made basic with 2N aqueous sodium hydroxide solution. The organic layer was separated, washed with water, and the solvent was evaporated under reduced pressure to give the title compound (0.27 g, 75%) as a white powder.

후처리

  1. temperaturewith heating
  2. concentrationThe reaction mixture was concentrated under reduced pressure, ethyl acetate
  3. additionwas added to the residue
  4. customThe organic layer was separated
  5. washwashed with water
  6. customthe solvent was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-0349a66488aa48f59f90d58cab307f0c
출처 데이터셋
uspto-grants-2013_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08470816B2

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