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Sodium Hydroxide → 6-Ethyl-3-oxo-n-(5-phenyl-2-pyrazinyl)spiro[isobenzofuran-1-(3h),4'-piperidine]-1'-carboxamide

HRID 990790
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인쇄 미리보기

반응식

HRID 990790 반응식
Cl.[CH2:2]([C:4]1[CH:17]=[C:16]2[C:7]([C:8](=[O:18])[O:9][C:10]32[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]3)=[CH:6][CH:5]=1)[CH3:3].[C:19]1([C:25]2[N:26]=[CH:27][C:28]([NH:31][C:32](=O)[O:33]C3C=CC=CC=3)=[N:29][CH:30]=2)[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1.[OH-].[Na+]>CS(C)=O>[CH2:2]([C:4]1[CH:17]=[C:16]2[C:7]([C:8](=[O:18])[O:9][C:10]32[CH2:11][CH2:12][N:13]([C:32]([NH:31][C:28]2[CH:27]=[N:26][C:25]([C:19]4[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=4)=[CH:30][N:29]=2)=[O:33])[CH2:14][CH2:15]3)=[CH:6][CH:5]=1)[CH3:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 9879110Phenyl 5-phenylpyrazin-2-ylcarbamateHCID 226607156-ethylspiro[isobenzofuran-1(3H),4'-piperidine]-3-one hydrochloride

생성물 1

HCID 226607536-Ethyl-3-oxo-n-(5-phenyl-2-pyrazinyl)spiro[isobenzofuran-1-(3h),4'-piperidine]-1'-carboxamide수율 54.2%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide
용매

실험 절차

To a suspension of 6-ethylspiro[isobenzofuran-1(3H),4′-piperidine]-3-one hydrochloride (53 mg) and phenyl N-(5-phenyl-2-pyrazinyl)carbamate (58 mg) in dimethyl sulfoxide (1 mL) was added 10 M sodium hydroxide aqueous solution (0.02 mL). The mixture was vigorously stirred for 5 minutes followed by partition between water and ethyl acetate. The organic layer was separated and then washed with saturated saline solution and then dried over anhydrous Na2SO4. The concentration of the organic solvent left a residue, which was subjected to the crystallization from ethyl acetate to give the subject compound (46 mg) as crystals (melting point 176-178° C.).

후처리

  1. customby partition between water and ethyl acetate
  2. customThe organic layer was separated
  3. washwashed with saturated saline solution
  4. dry with materialdried over anhydrous Na2SO4
  5. waitThe concentration of the organic solvent left a residue, which
  6. customwas subjected to the crystallization from ethyl acetate

출처 및 근거

ORD 기록
ord-a65750f9e4bd42cb83bc6c2b9cc11c01
출처 데이터셋
uspto-grants-2002_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06462053B1

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