Potassium Carbonate → HCID 22508909, 화합물

HRID 1163055노트

반응식

HRID 1163055 반응식
[F:1][C:2]1[C:10]([O:11][C:12]2[C:17]3=[C:18]([CH3:26])[C:19]([O:21][CH2:22][CH:23]4[CH2:25][O:24]4)=[CH:20][N:16]3[N:15]=[CH:14][N:13]=2)=[CH:9][CH:8]=[C:7]2[C:3]=1[CH:4]=[C:5]([CH3:27])[NH:6]2.[CH3:28][N:29]([CH3:34])[S:30]([NH2:33])(=[O:32])=[O:31].[C:35](=O)([O-])[O-].[K+].[K+]>CN(C=O)C.ClCCl>[F:1][C:2]1[C:10]([O:11][C:12]2[C:17]3=[C:18]([CH3:26])[C:19]([O:21][CH2:22][CH:23]([OH:24])[CH2:25][CH2:35][NH:33][S:30]([N:29]([CH3:34])[CH3:28])(=[O:32])=[O:31])=[CH:20][N:16]3[N:15]=[CH:14][N:13]=2)=[CH:9][CH:8]=[C:7]2[C:3]=1[CH:4]=[C:5]([CH3:27])[NH:6]2

참가 물질

6

반응물 3

HCID 11430Potassium CarbonateHCID 134472N,N-DimethylsulfamideHCID 22508879HCID 22508879, 화합물

생성물 1

HCID 22508909HCID 22508909, 화합물수율 25%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 6344Dichloromethane용매

실험 절차

A mixture of Example 2 (40 mg, 0.11 mmol), N,N-dimethylsulfamide (94 mg, 0.66 mmol) and potassium carbonate (91 mg, 0.66 mmol) in DMF (0.5 ml) was stirred at 80° C. for 1.5 h. The mixture was diluted with dichloromethane, filtered and concentrated in vacuo. The crude material was purified by preparative HPLC, followed by chromatography on silica gel eluting with 10% methanol in ethyl acetate to afford the title compound (13.7 mg, 25% yield) as a white solid. MS: (M+H)+=493.1

후처리

  1. filtrationfiltered
  2. concentrationconcentrated in vacuo
  3. customThe crude material was purified by preparative HPLC

출처 및 근거

ORD 기록
ord-f0be806b552548c2a1945fc6406bfa88
출처 데이터셋
uspto-grants-2010_10
특허 번호
US07820814B2

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