Water → HCID 59517316, 화합물

HRID 1698643노트

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HRID 1698643 반응식
[NH4+]=[S:2].[Si:3]([O:10][C:11]1[CH:16]=[CH:15][C:14]([CH:17]([NH:20][C:21]2[CH:26]=[CH:25][C:24]([C:27]3[N:31]=[C:30]([CH3:32])[O:29][N:28]=3)=[CH:23][CH:22]=2)[C:18]#[N:19])=[CH:13][C:12]=1[O:33][CH3:34])([C:6]([CH3:9])([CH3:8])[CH3:7])([CH3:5])[CH3:4].C1COCC1.O>CO.C(OCC)(=O)C>[Si:3]([O:10][C:11]1[CH:16]=[CH:15][C:14]([CH:17]([NH:20][C:21]2[CH:22]=[CH:23][C:24]([C:27]3[N:31]=[C:30]([CH3:32])[O:29][N:28]=3)=[CH:25][CH:26]=2)[C:18]([NH2:19])=[S:2])=[CH:13][C:12]=1[O:33][CH3:34])([C:6]([CH3:9])([CH3:8])[CH3:7])([CH3:4])[CH3:5]

참가 물질

6

반응물 3

HCID 962WaterHCID 8028TetrahydrofuranHCID 59516853HCID 59516853, 화합물

생성물 1

HCID 59517316HCID 59517316, 화합물

시약·촉매·용매 2

HCID 887Methanol용매HCID 8857Ethyl Acetate용매

실험 절차

After adding 32 ml of a 20% aqueous solution of ammonium sulfide to a solution of 8.45 g of (4-t-butyldimethylsilanyloxy-3-methoxyphenyl)-[4-(5-methyl-[1,2,4]oxadiazol-3-yl)phenylamino]acetonitrile in 300 ml of a methanol:THF=2:1 mixed solvent, the mixture was stirred at room temperature for 23 hours. Water was added to the reaction mixture and extraction was performed with ethyl acetate. After washing the organic layer with saturated brine, it was dried over anhydrous sodium sulfate. The desiccating agent was filtered off, and the filtrate was concentrated under reduced pressure to give the title compound (8.26 g) as a crude product.

후처리

  1. washAfter washing the organic layer with saturated brine, it
  2. dry with materialwas dried over anhydrous sodium sulfate
  3. filtrationThe desiccating agent was filtered off
  4. concentrationthe filtrate was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-ee3191d3d70d4346b056b3e289a1c170
출처 데이터셋
uspto-grants-2012_04
특허 번호
US08163787B2

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