Water → HCID 178434789、化合物

HRID 2246292ノート

反応式

HRID 2246292 の反応式
[SH:1][C:2]1[NH:6][CH:5]=[N:4][N:3]=1.Cl[C:8]1[CH:9]=[CH:10][C:11]2[N:12]=[CH:13][N:14]=[C:15]([NH:18][C:19]3[S:23][N:22]=[C:21]([CH3:24])[N:20]=3)[C:16]=2[N:17]=1.C(O[K])(C)(C)C.O>CN(C)C(=O)C>[N:4]1[N:3]=[C:2]([S:1][C:8]2[CH:9]=[CH:10][C:11]3[N:12]=[CH:13][N:14]=[C:15]([NH:18][C:19]4[S:23][N:22]=[C:21]([CH3:24])[N:20]=4)[C:16]=3[N:17]=2)[NH:6][CH:5]=1

参加物

6

反応物 4

HCID 962WaterHCID 23160294(6-Chloro-pyrido[3,2-d]pyrimidin-4-yl)-3-methyl-[1,2,4]thiadiazol-5-yl-amineHCID 178418922HCID 178418922、化合物HCID 178527972HCID 178527972、化合物

生成物 1

HCID 178434789HCID 178434789、化合物収率 2.4%

試薬・触媒・溶媒 1

HCID 31374Dimethylacetamide溶媒

反応条件

温度
130 °C

実験手順

3-Mercapto-4H-[1,2,4]triazole (54 mg; 0.54 mmol) and 100 mg (0.36 mmol) of (6-chloro-pyrido[3,2-d]pyrimidin-4-yl)-3-methyl-[1,2,4]thiadiazol-5-yl-amine were added to a solution of 80 mg (0.72 mmol) of tert-butoxy potassium in 3 ml of N,N-dimethylacetamide and the mixture was stirred at 130° C. for 16 hours. Water was added to the reaction solution and the mixture was extracted with chloroform. The organic layer was dried and concentrated and the resulting residue was purified by a reversed phase preparative HPLC (0.1% TFA-containing water:acetonitrile=90:10→10:90) to give 3 mg (yield: 2%) of the title compound as a yellow solid.

後処理

  1. extractionthe mixture was extracted with chloroform
  2. customThe organic layer was dried
  3. concentrationconcentrated
  4. customthe resulting residue was purified by a reversed phase preparative HPLC (0.1% TFA-containing water:acetonitrile=90:10→10:90)

出典と根拠

ORDレコード
ord-9e2d96fd6e9d44998cdf65a2f93b4a92
出典データセット
uspto-grants-2010_03
特許番号
US07687502B2

反応ノート

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