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Potassium Carbonate → HCID 474117, 화합물

HRID 963528
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HRID 963528 반응식
[C:1]1([CH2:7][C:8]([C@H:10]2[C@@H:14]([C:15](=O)[CH2:16][C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=3)[N:13]([CH2:24][C:25]3[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=3)C(=O)[N:11]2[CH2:32][C:33]2[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=2)=[O:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C([O-])(=O)C.[NH4+].[C:44](=[O:47])([O-])[O-].[K+].[K+]>C(O)(=O)C>[CH2:24]([N:13]1[C:14]2=[C:15]([CH2:16][C:17]3[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=3)[O:9][C:8]([CH2:7][C:1]3[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=3)=[C:10]2[N:11]([CH2:32][C:33]2[CH:34]=[CH:35][CH:36]=[CH:37][CH:38]=2)[C:44]1=[O:47])[C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 517165Ammonium AcetateHCID 70072032HCID 70072032, 화합물

생성물 1

HCID 474117HCID 474117, 화합물수율 76%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

A solution of (4R-cis)-4,5-bis(phenylacetyl)-1,3-bis(benzyl)-2-imidazolidinone (79 mg, 0.16 mmol) and ammonium acetate (25 mg, 0.32 mmol) in acetic acid (2 ml) was refluxed 18 hours. The solution was neutralized with solid potassium carbonate and partitioned between EtOAc/water. The aqueous phase was washed twice with EtOAc. All organic extracts were combined and dried over MgSO4, then concentrated to a brown oil. Further purification was achieved by preparative TLC (silica gel, 30% EtOAc/hexane) to give the product as a yellow-brown oil, (59 mg, 76% yield). 1HNMR (CDCl3) δ7.10-7.44 (m, 10H), 4.99-5.16 (m, 2H) , 4.17-4.29 (m, 3H), 3.59 (d, 1H), 2.54 (m, 1H), 2.07-2.33 (m, 3H), 1.21-1.50 (m, 6H), 0.84-0.93 (m, 6H). MS: 417 (M+1).

후처리

  1. custompartitioned between EtOAc/water
  2. washThe aqueous phase was washed twice with EtOAc
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated to a brown oil
  5. customFurther purification

출처 및 근거

ORD 기록
ord-a6a03a56748a46e7b532107a3577ca17
출처 데이터셋
uspto-grants-1998_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05763469

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