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Fumaric Acid → N-[(6R,7S)-7-(3,4-dichlorophenyl)-1,4-oxazepan-6-yl]acetamide monofumarate

HRID 1022621
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HRID 1022621 반응식
[C:1]([NH:4][C@H:5]1[C@H:11]([C:12]2[CH:17]=[CH:16][C:15]([Cl:18])=[C:14]([Cl:19])[CH:13]=2)[O:10][CH2:9][CH2:8][N:7](C(OC(C)(C)C)=O)[CH2:6]1)(=[O:3])[CH3:2].C(OCC)(=O)C.Cl.[C:34]([OH:41])(=[O:40])/[CH:35]=[CH:36]/[C:37]([OH:39])=[O:38]>C(O)C>[C:34]([OH:41])(=[O:40])/[CH:35]=[CH:36]/[C:37]([OH:39])=[O:38].[Cl:19][C:14]1[CH:13]=[C:12]([C@@H:11]2[O:10][CH2:9][CH2:8][NH:7][CH2:6][C@H:5]2[NH:4][C:1](=[O:3])[CH3:2])[CH:17]=[CH:16][C:15]=1[Cl:18]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 444972Fumaric AcidHCID 21866389Hydrogen chloride-ethyl acetateHCID 66975754tert-butyl (6R,7S)-6-(acetylamino)-7-(3,4-dichlorophenyl)-1,4-oxazepane-4-carboxylate

생성물 1

HCID 86663854N-[(6R,7S)-7-(3,4-dichlorophenyl)-1,4-oxazepan-6-yl]acetamide monofumarate수율 106.8%

시약·촉매·용매 1

HCID 702Ethanol
용매

실험 절차

To tert-butyl (6R,7S)-6-(acetylamino)-7-(3,4-dichlorophenyl)-1,4-oxazepane-4-carboxylate (200 mg) was added 4.0 M hydrogen chloride-ethyl acetate solution (4 mL), and the mixture was stirred at room temperature for 1 hr. The residue obtained by concentration under reduced pressure was desalted by a solid phase extraction resin (column: PL StrastoSphere solid phase extraction resin (PL-HCO3 MP StratoSpheres™), 500 mg, StrastoSphere, mobile phase: methanol). To a solution of the residue obtained by concentration under reduced pressure in ethanol was added a solution of fumaric acid (33.7 mg) in ethanol. The mixture was concentrated under reduced pressure to give the title compound (130 mg).

후처리

  1. customThe residue obtained by concentration under reduced pressure
  2. extractionwas desalted by a solid phase extraction resin (column
  3. extractionPL StrastoSphere solid phase extraction resin (PL-HCO3 MP StratoSpheres™), 500 mg
  4. customTo a solution of the residue obtained by concentration under reduced pressure in ethanol
  5. concentrationThe mixture was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-8aa8d611b2354113bb13f33cf758fbdb
출처 데이터셋
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08722662B2

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