Water → HCID 59517316、化合物

HRID 1161395ノート

反応式

HRID 1161395 の反応式
[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]

参加物

6

反応物 3

HCID 962WaterHCID 8028TetrahydrofuranHCID 59516853HCID 59516853、化合物

生成物 1

HCID 59517316HCID 59517316、化合物

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-6be77722172e44e79afd749689858160
出典データセット
uspto-grants-2010_10
特許番号
US07816522B2

反応ノート

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